- The liquid containing β - halohydrin of the isolation of the product of the method
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The present invention relates to a liquid containing β - process for the isolation of the product of the method, the method comprises: a, β - halo containing liquid product after mixing with the organic extractant extraction, the aqueous phase and the oil phase obtained; b, a distillation step obtained states the oil phase, to obtain the β - halohydrin; the organic extractant comprises a 1st component and 2nd component, the 1st group is divided into not substituted alkanes and/or not substituted olefin, the 2nd group [...] substituted alkanes and/or Cl substituted olefin, the 1st component 2nd component and the molar ratio of 1: (0.05 - 3). The method of simple process flow, low energy consumption, and can separate to obtain a high purity of the halohydrin β -.
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Paragraph 0103-0106; 0115-0122; 0131
(2019/05/16)
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- ATG7 INHIBITORS AND THE USES THEREOF
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Disclosed are chemical entities which are compounds of formula (I) : or a pharmaceutically acceptable salt thereof, wherein R1, R2, and Ra have the values described herein. Chemical entities according to the disclosure can be useful as inhibitors of ATG7. Further provided are pharmaceutical compositions comprising a chemical entity of the disclosure and methods of using the compositions in the treatment of cancer.
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Paragraph 00399; 00401
(2018/05/27)
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- Method for preparing halogen propanol and epoxypropane
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The invention provides a method for preparing halogen propanol. The method comprises the following steps (1) halogen alcoholization: adding halogen hydride, H2O2, propylene and an HTS molecular sieve into a reaction device, and carrying out halogen alcoholization reaction to obtain the halogen propanol. The invention also provides a method for preparing epoxypropane with a halogenohydrin method. The method comprises the following steps: (1) halogen alcoholization: adding halogen hydride, H2O2, propylene and an HTS molecular sieve into the reaction device, and carrying out the halogen alcoholization reaction to obtain halogen propanol; (2) saponification: carrying out saponification reaction on halogen propanol and a hydroxide of alkali metal in step (1), and separating to obtain the epoxypropane and alkali halide metal salt; optionally (3) electroosmosis: carrying out bipolar membrane electroosmosis on the alkali halide metal salt obtained in step (2) to obtain the hydroxide of alkali metal and the halogen hydride. According to the methods, the halogen propanol or the epoxypropane can be prepared at extremely high selectivity and yield, and the discharging of waste water and waste residues can be drastically lowered.
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Paragraph 0086; 0087-0099; 0104; 0105; 0112-0115; 0118-0130
(2017/05/19)
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- A convenient method for producing mono- and dichlorohydrins from glycerol
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A new method for the transformation of glycerol into mono- and dichlorohydrins has been studied. With trimethylchlorosilane as chlorinating agent and acetic acid as catalyst, mono- and dichlorohydrins have been obtained in high yields and selectivity. In fact, under different reaction conditions, the synthesis of α-monochlorohydrin (3-chloropropan-1,2-diol) or α,γ-dichlorohydrin (1,3-dichloropropan-2-ol) as predominant product has been achieved. This process was also exploited for the valorisation of the crude mixture of glycerol and monochlorohydrin (glyceric mixture), a by-product from an earlier BioDiesel production. A reaction mechanism has been proposed based on investigations on the chlorination of different alcohols.
- Giomi, Donatella,Malavolti, Marino,Piccolo, Oreste,Salvini, Antonella,Brandi, Alberto
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p. 46319 - 46326
(2015/02/19)
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- Dehydrochlorination of 2-chloroethanol, 2-chloro-1-propanol, 1-chloro-2-propanol, 2-chloro-2-methyl-1-propanol and 1-chloro-2-methyl-2- propanol
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The reactions between a few 1,2-chlorohydrins and sodium hydroxide have been studied and shown to involve a two-step nucleophilic elimination of hydrogen chloride. The data are given for the slow rate-determining step of 2-chloroethanol 1, 2-chloro-1-propanol 2, 1-chloro-2- propanol 3, 2-chloro-2-methyl-1-propanol 4 and 1-chloro-2-methyl-2-propanol 5. Compounds 4 and 5 gave 2-methyl-1,2-propanediol as the final product instead of oxiranes given by compounds 13. In contrast to some earlier reports the mere water reaction was shown to be almost negligible. In constant ionic strength the base concentration had no effect on the rates whereas at different base concentrations (0.0500.250 mol dm-3) alone the rate of alkaline dehydrochlorination of 1 clearly decreased (103k2, dm 3 mol-1 s-1: 10.0-8.7, respectively). The rate of 2 at constant base concentration (0.010 mol dm-3) and at different ionic strengths (dm3 mol-1: 0.010-0.500) decreased also (103k2, dm3 mol-1 s-1: 76-65, respectively) indicating that the decrease is mainly due to the change in the ionic strength also in the former case. ARKAT-USA, Inc.
- Pihlaja, Kalevi,Kiuru, Marja-Leena,Sippola, Anne
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p. 120 - 133
(2013/09/24)
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- The reactions of 4-chloro-2-butanol and 3-chloro-1-butanol with aqueous sodium hydroxide, and 1-chloro-2-propanol and 2-chloro-1-propanol with isopropyl amine
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The total reaction of 4-chloro-2-butanol 1 with NaOH(aq) is dominated (74%) by intramolecular substitution (SNi), besides which bimolecular substitution (SN2, 12%) and 1,4-elimination (i.e. fragmentation, contrary to earlier arguments) exhibit a significant contribution (11%). The total reaction of 3-chloro-1-butanol 2 instead is dominated by 1,4-(72%) and 1,2-elimination (25%), the substitution reactions being just observable (SNi 2% and SN2 1%). In 1 both the +I-effect and the conformational factors in the intermediate γ-chloroalkoxy anion favour the SNi-reaction, whereas in 2 the situation is opposite and the location of Cl on a secondary carbon also makes the SNi-reaction less favourable. The relative proportions of 1,4-and 1,2-eliminations for 2 can be explained by thermodynamic basis since the consequent products are more stable than the corresponding products from 1. 1-chloro-2-propanol 3 and 2-chloro-1-propanol 4 both react with isopropyl amine giving the same product, namely 1-isopropylamino-2-propanol, which indicates that the reaction proceeds through the propylene oxide intermediate. Compound 1 also reacted with isopropyl amine predominantly via SNi-reaction, giving first 2-methyloxetane which then further gave 4-isopropylamino-2-butanol, whereas 2 gave 3-isopropylamino-1-butanol through a direct S N2-reaction. ARKAT-USA, Inc.
- Pihlaja, Kalevi,Aaljoki, Kari,Lyytinen, Maija-Riitta,Huusko, Marja-Liisa,Hotokka, Marjut
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experimental part
p. 188 - 199
(2011/07/07)
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- Asymmetric alkyl-alkyl cross-couplings of unactivated secondary alkyl electrophiles: Stereoconvergent suzuki reactions of racemic acylated halohydrins
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A method for asymmetric alkyl-alkyl Suzuki reactions of unactivated secondary alkyl electrophiles, specifically, cross-couplings of racemic acylated halohydrins with alkylborane reagents, has been developed. A range of protected bromohydrins, as well as a protected chlorohydrin and a homologated bromohydrin, are coupled in good ee by a catalyst derived from commercially available components.
- Owston, Nathan A.,Fu, Gregory C.
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supporting information; experimental part
p. 11908 - 11909
(2010/11/04)
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- Synthesis of oxygen-containing spirobipyrrolidinium salts for high conductivity room temperature ionic liquids
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Synthesis of ionic liquids (IL) based on oxygen-containing spirobipyrrolidinium salts with BF4 , BF3C 2F5 , and NTf2 as counterions was undertaken. Their physical and electrochemical properties were evaluated for suitability for Room Temperature Ionic Liquids (RTIL) application. Reduction in melting point occurred upon exchange of C(2) by an O-atom of spirobipyrrolidinium, without sacrificing the electrochemical stability; while introduction of alkyl groups between the N- and O-atoms led to incorporation of asymmetry, and hence reduced the melting points, and viscosity.
- Higashiya, Seiichiro,Devarajan, Thamarai Selvi,Rane-Fondacaro, Manisha V.,Dangler, Christopher,Snyder, Jeremy,Haldar, Pradeep
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experimental part
p. 1600 - 1609
(2009/10/16)
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- CONVERSION OF A MULTIHYDROXYLATED-ALIPHATIC HYDROCARBON OR ESTER THEREOF TO A CHLOROHYDRIN
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The present invention relates to a process for converting a multihydroxylated-aliphatic hydrocarbon or ester thereof to a chlorohydrin, by contacting the multihydroxylated-aliphatic hydrocarbon or ester thereof starting material with a source of a superatmospheric partial pressure of hydrogen chloride for a sufficient time and at a sufficient temperature, and wherein such contracting step is carried out without substantial removal of water, to produce the desired chlorohydrin product; wherein the desired product or products can be made in high yield without substantial formation of undesired overchlorinated byproducts. In addition, certain catalysts of the present invention may be used in the present process at superatmospheric, atmospheric and subatmospheric pressure conditions with improved results.
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Page/Page column 37-38
(2008/06/13)
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- Synthesis and extractive power of alkyl-substituted 1,4-dithiane derivatives
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The reactions of β,β'-dichlorodialkyl sulfides and β,β'-dichlorodialkyl sulfones with Na2S and Na2S2 were studied, and the extraction power of the reaction products with respect to Au(III) and Pd(II) was examined.
- Krivonogov,Afzaletdinova,Khisamutdinov,Spirikhin,Murinov
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p. 1036 - 1042
(2007/10/03)
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- Synthesis of Oxochromium(VI) Alkoxides via Epoxide Cleavage. Structure, Reactivity, and Mechanism
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In an NMR spectroscopic study the cleavage of epoxides [ethylene, propylene, and cis/trans-butylene oxide] by chromyl chloride giving access to oxochromium(VI) alkoxides was shown to proceed via a bimolecular rate-determining step where two molecules of a complex CrO2Cl2...epoxide collide. Subsequently one Cl ligand at the first Cr center attacks the backside of an epoxide molecule complexed at the Cr center of a second CrO2Cl2...epoxide molecule and vice versa. The trans-opening of the epoxides was proved by determining the configuration of the chlorohydrins resulting from hydrolysis of the corresponding alkoxide products in the cases of cis- and trans-butylene oxide. The NMR data provide evidence that each oxochromium(VI) alkoxide adopts one preferred conformation in solution although DFT calculations did not indicate any special stabilizing effects. The product formation was rationalized by DFT calculations concerning the thermodynamics of the reactions.
- Limberg, Christian,Wistuba, Tobias
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p. 6169 - 6176
(2007/10/03)
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- Highly regio- and stereoselective synthesis of β-halohydrins from epoxides catalyzed with ceric ammonium nitrate
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Ce(IV) as ceric ammonium nitrate can effectively catalyze ring opening of epoxides with halides under very mild conditions and easy procedure to give the corresponding β-chloro- and β-bromohydrins in excellent yields. The reactions occur with both substituted and unsubstituted quaternary ammonium halides and with high regio- and stereoselectivity. The reaction of optically active styrene oxide with chloride ion was found to be highly stereospecific and afforded the corresponding β-halohydrin in 96% ee.
- Iranpoor,Kazemi,Salehi
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p. 1247 - 1258
(2007/10/03)
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- Highly Regioselective and Stereospecific Functionalization of 1,2-Proanediol with Trimethyl(X)silanes Employing the 1,3,2λ5-Dioxaphospholane Methodology
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The regioselective ring opening of (S)-4-methyl-2,2,2-triphenyl-1,3,2λ5-dioxaphospholanes (2) was initiated with several trimethylsilyl reagents (Me3SiX: X = PhS, I, Br; Cl, CN, and N3) to afford the regioisomeric (silyloxy)phosphonium salts.A stereospecific extrusion of triphenylphosphine oxide from these oxyphosphonium salts gave predominatly the thermodynamically less stable C-2-X-substituted derivatives with nearly complete inversion of stereochemistry at the C-2 stereogenic center (i.e., X = PhS).
- Mathieu-Pelta, Isabel,Evans, Slayton A.
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p. 3409 - 3413
(2007/10/02)
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- SYNTHESIS AND THERMAL PROPERTIES OF SIDE CHAIN TYPE LIQUID CRYSTALLINE POLYMERS WITH CHIRAL UNIT IN THE FLEXIBLE MOIETY
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This paper is concerned with the synthesis and thermal properties for five families of side-chain type liquid crystalline polymers.All these side-chain type polymers showed an enantiotropic mesomorphic nature.A sharp reflexion was observed in the small angle region, whereas a broad halo or a relatively sharp peak was also detected in the wide angle region for all the polymers.The experimental values of the thickness of the smectic layer which can be easily assigned by the polarizing microscopic measurements were smaller than that of the calculated ones.This difference would be caused from the tilted arrangement in the smectic layer or smectic A like structure in which the side chain would be overlapped.
- Koide, Naoyuki,Uehara, Keiichi,Iimura, Kazuyoshi
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p. 151 - 162
(2007/10/02)
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- HETEROGENEOUS ASYMMETRIC RING-OPENING REACTIONS OF PROCHIRAL EPOXIDES INCLUDED AS GUEST MOLECULES IN TRI-o-THYMOTIDE CLATHRATES.
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Enantiomorphous tri-o-thymotide clathrates of prochiral oxiranes were submitted to the action of gaseous hydrogen halides.Ring-opening reactions ensued that differ from those reported in homogeneous phase, showing a considerable modification of the chemical reactivity of the external reagent in the host lattice.Chirality transfer from the host receptors to the guest products was also observed, but with a poor efficiency.
- Gerdil, Raymond,Barchietto, Giacomo
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p. 4685 - 4688
(2007/10/02)
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- THERMAL CONVERSIONS OF alpha -PROPYLENE CHLOROHYDRIN.
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The purpose of the authors' work was to determine the principal relationships of thermal decomposition of anhydrous PCH in the liquid phase. Preliminary experiments showed that appreciable decomposition of PCH begins only at 130 degree . Therefore thermal conversions of PCH were studied at higher temperatures than in the case of ethylene chlorohydrin in the range 140-170 degree . It is shown that acetone, 1-(1-chloroisopropoxy)-2-propanol, 2-chloro-1-propanol, hydrogen chloride, and 1,2-dichloropropane are formed during liquid-phase thermal decomposition of 1-chloro-2-propanol in the temperature range 140-170 degree . Isomerization of 1-chloro-2-propanol to 2-chloro-1-propanol is accelerated by the hydrogen chloride formed during its thermal decomposition.
- Kolesnikov,Zil'berman,Danov,Efremov
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p. 2384 - 2386
(2007/10/02)
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- Cyclodehydration and Chlorination of Simple Diols with Triphenylphosphine and tert-Butyl Hypochlorite
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The reagent triphenylphosphine-tert-butyl hypochlorite converts 1,4-diols into the corresponding tetrahydrofurans and 1,2-diols into a mixture of the regioisomeric chlorohydrins and the epoxides at -78 deg C followed by warming to ambient temperature (ca. 30 deg C).Symmetrical diols give largely chlorohydrins and dichlorides.
- Barry, Carey N.,Evans, Slayton A.
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p. 2825 - 2828
(2007/10/02)
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- Studies on the Mechanism of the Chlorohydrination of Olefins
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We studied the rate-determining and the product-determining steps of the chlorohydrination of olefins with Cl2/H2O and HOCl.In competitive kinetic experiments with 3-ethylpent-2-ene and cyclohexene we determined the relative rate constants krel=1,5 (with Cl2/H2O) and krel=infinite (with HOCl).This shows that the rate-determining steps of the chlorohydrination with Cl2/H2O and with HOCl are different.In order to investigate the product-determining steps we determined the proportion of alkyl-(2-chloroethyl)-ethers 3 and ethylene chlorohydrine 2 in the reaction of ethylene with Cl2 and with HOCl in alcohol/water-mixtures.The proportion of both the reaction products 3/2 was independent of the chlorinating agent used.Also the proportion of MARKOVNIKOV and anti-MARKOVNIKOV products in the chlorohydrination of propylene with Cl2/H2O or HOCl was independent of the type of chlorinating agent.In the chlorohydrination of cyclohexene both agents (Cl2/H2O and HOCl) yielded only the trans-chlorohydrine.From the results obtained it may be concluded that the product-determining step of chlorohydrination is the same for both the chlorinating agents studied.
- Buss, E.,Rockstuhl, A.,Schnurpfeil, D.
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p. 197 - 208
(2007/10/02)
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