- Preparation method of aminobutyronitrile
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The invention discloses a preparation method of aminobutyronitrile, which comprises the following steps: mixing ammonia water with ammonium bicarbonate and methyl isobutyl ketone, adding sodium cyanide, dropwisely adding n-propionaldehyde, carrying out heat preservation reaction, conducting standing for stratification after the reaction is finished, and concentrating the organic phase to remove the solvent, thereby obtaining aminobutyronitrile. According to the method, the raw materials are easy to obtain, the reaction conditions are environmentally friendly and safe, the reaction time is short, the solvent can be recycled, the steps are simple, and the obtained product has high purity.
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Paragraph 0022-0034
(2021/02/10)
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- Method for preparing 2-aminobutyronitrile through microchannel reactor
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The invention provides a method for preparing 2-aminobutyronitrile through a microchannel reactor. The method includes: with a NaCN/ammonia/NH4Cl/water mixed solution as a first material and n-propanal as a second material, feeding the raw materials into the microchannel reactor, and performing continuous flow synthesis at 10-40 DEG C to prepare the 2-aminobutyronitrile, reaction time being 5-40 sand pressure being 0-15 bar. Compared with a common kettle reactor in the prior art, the method is short in reaction time, is low in liquid holdup volume, is low in impurity and high in yield, is free of amplification effect, is greatly improved in safety and controllability than the kettle reactor, is beneficial to continuous automatic control, and improves production efficiency.
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Paragraph 0025-0041
(2020/04/17)
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- Production system of 2-aminobutanamide
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The utility model provides a production system of 2-aminobutanamide, which comprises a first reactor, a second reactor, a third reactor, a fourth reactor, a fifth reactor and a sixth reactor, the second reactor is communicated with the first reactor and is used for reacting 2-hydroxybutyronitrile with an ammonia source to prepare 2-aminobutyronitrile; the third reactor is communicated with the second reactor and is used for carrying out hydrolysis reaction on the 2-aminobutyronitrile and strong base to prepare the 2-aminobutyramide. The device effectively reduces waste water, waste gas and waste residues, effectively reduces the use amount of hydrogen cyanide, improves the content of target products, and reduces the production cost.
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Paragraph 0069; 0093; 0094; 0107-0113
(2020/04/17)
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- Preparation method of (S)-(+)-2-aminobutanamide hydrochloride
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The invention discloses a synthetic process of a chiral drug (S)-alpha-ethyl-2-oxo-pyrrolidine acetamide (levetiracetam) intermediate (S)-(+)-2-aminobutanamide hydrochloride which has anti-epileptic function. The synthetic process comprises the following steps: performing condensation on acetone cyanohydrins and n-propanal as initial raw materials in the presence of a catalyst to obtain 2-hydroxybutyronitrile; then carrying out a reaction with ammonia to obtain 2-amino butyronitrile; then carrying out hydrolysis to obtain 2-aminobutanamide; then splitting and salifying the 2-aminobutanamide to obtain a target product. The synthetic process is high in yield, the raw materials are low in price and are easily purchased on a large scale, and the synthetic process overcomes the defects that several existing processes need highly toxic and highly polluting raw materials and is simple in process operation and low in cost. Mother liquor after splitting is further racemized and split and is recycled repeatedly, so that the synthetic process is suitable for industrial production.
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Paragraph 0035; 0036; 0037
(2019/01/23)
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- Preparation method and preparation system of 2-aminobutyramide
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The invention provides a preparation method and a preparation system of 2-aminobutyramide. The preparation method comprises: (1) generating 2-hydroxybutyronitrile from hydrogen cyanide and n-propanalunder the action of a first catalyst; (2) adding an ammonia source and a second catalyst to the 2-hydroxybutyronitrile obtained in the step (1), and carrying out a reaction to generate 2-aminobutyronitrile; and (3) removing the excess ammonia from the reaction solution obtained in the step (2), adding a strong base and a third catalyst, and carrying out a hydrolysis reaction to obtain DL-2-aminobutanamide. According to the present invention, with the method and the system, the wastewater, the waste gas and the waste residue can be effectively reduced, the consumption of hydrogen cyanide can beeffectively reduced, the content of the target product can be increased, and the production cost can be reduced.
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Paragraph 0091; 0092-0110
(2019/10/01)
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- A process for preparing 2 - amino ding amide hydrochloride
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The invention discloses a method for preparing 2-aminobutanamide hydrochloride. The method comprises the following steps of: reacting 2-aminobutyronitrile with aromatic aldehyde in an alkaline aqueous solution to generate corresponding Schiff base; and hydrolyzing the obtained Schiff base under an acidic condition to obtain 2-aminobutanamide hydrochloride. According to the method disclosed by the invention, the product quality is good, the method is simple to operate, the aftertreatment is convenient, and the process is environment-friendly and is beneficial to industrial production.
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Paragraph 0022; 0023
(2018/03/01)
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- Prebiotic selection and assembly of proteinogenic amino acids and natural nucleotides from complex mixtures
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A central problem for the prebiotic synthesis of biological amino acids and nucleotides is to avoid the concomitant synthesis of undesired or irrelevant by-products. Additionally, multistep pathways require mechanisms that enable the sequential addition of reactants and purification of intermediates that are consistent with reasonable geochemical scenarios. Here, we show that 2-aminothiazole reacts selectively with two- and three-carbon sugars (glycolaldehyde and glyceraldehyde, respectively), which results in their accumulation and purification as stable crystalline aminals. This permits ribonucleotide synthesis, even from complex sugar mixtures. Remarkably, aminal formation also overcomes the thermodynamically favoured isomerization of glyceraldehyde into dihydroxyacetone because only the aminal of glyceraldehyde separates from the equilibrating mixture. Finally, we show that aminal formation provides a novel pathway to amino acids that avoids the synthesis of the non-proteinogenic α,α-disubstituted analogues. The common physicochemical mechanism that controls the proteinogenic amino acid and ribonucleotide assembly from prebiotic mixtures suggests that these essential classes of metabolite had a unified chemical origin.
- Islam, Saidul,Bu?ar, Dejan-Kre?imir,Powner, Matthew W.
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p. 584 - 589
(2017/05/31)
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- Preparation method for levetiracetam intermediate L-2-aminobutanamide hydrochloride
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The invention relates to a preparation method for a levetiracetam intermediate L-2-aminobutanamide hydrochloride. The method comprises the steps that n-propanal reacts with ammonia and hydrocyanic acid in a water solution under existing of ammonium chloride to prepare 2-amidogen butyronitrile, a certain amount of liquid ammonia and hydrocyanic acid are fed into mother liquor, and the mother liquor can be used indiscriminately for infinite times; the 2-amidogen butyronitrile is hydrolyzed in a 1% sodium hydroxide water solution to obtain 2-aminobutanamide, and water can be used indiscriminately for infinite times after being distilled; the 2-aminobutanamide is subjected to resolution to obtain L-2-aminobutanamide; salifying is carried out, and the L-2-aminobutanamide hydrochloride is obtained. The method has the advantages that the product quality is good, no waste water is produced in the production process, and the cost is low, and the preparation method is suitable for industrial production.
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Paragraph 0044; 0047; 0048; 0056; 0057; 0065; 0066
(2017/04/18)
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- Preparation method of S-2-aminobutanamide
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The invention provides a preparation method of S-2-aminobutanamide, comprising the steps of 1), reacting hydrogen cyanide, ammonia and n-propanal as materials to obtain 2-aminobutanenitrile; 2), separating a reacted liquid of step 1) by means of extraction to obtain an oil phase and a water phase, adding a catalyst and an alkali solution into the oil phase to carrying out hydrolysis, and reacting to obtain hydrolysate; 3), adding an acid or acid aqueous solution into the hydrolysate of step 2), separating to obtain an oil phase and a water phase, and separating the water phase to obtain S-2-aminobutanamide. The hydrogen cyanide, n-propanal and ammonia are reacted as materials to synthesize 2-aminobutanenitrile, the 2-aminobutanenitrile is hydrolyzed to directly obtain a target product, little byproducts are produced in reaction, and the content of the target product is high; little waste water and waste gas are produced in reaction, zero residue is produced, and there is no mass waste salts produced in the sodium cyanide process; the operation is simple, and product yield and purity are high.
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Paragraph 0025; 0026; 0030; 0031
(2017/02/09)
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- Radiosynthesis of 11C-levetiracetam: A potential marker for PET imaging of SV2A expression
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The multistep preparation of 11C-levetiracetam (11C-LEV) was carried out by a one-pot radiosynthesis with 8.3 ± 1.6% (n = 8) radiochemical yield in 50 ± 5.0 min. Briefly, the propionaldehyde was converted to propan-1-imine in situ as labeling precursor by incubation with ammonia. Without further separation, the imine was reacted with 11C-HCN to form 11C-aminonitrile. This crude was then reacted with 4-chlorobutyryl chloride and followed by hydrolysis to yield 11C-LEV after purification by chiral high-performance liquid chromatography (HPLC). Both the radiochemical and enantiomeric purities of 11C-LEV were >98%.
- Cai, Hancheng,Mangner, Thomas J.,Muzik, Otto,Wang, Ming-Wei,Chugani, Diane C.,Chugani, Harry T.
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supporting information
p. 1152 - 1155
(2014/12/10)
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- The CSIC reaction on substrates derived from aldehydes
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The Carbanion-mediated Sulfonate (Sulfonamide) Intramolecular Cyclization reaction (CSIC reaction) on conveniently functionalized cyanoalkylsulfonates and cyanoalkylsulfonamides derived from aldehydes is possible and gives the new heterocyclic ring systems 5-alkyl-4-amino-5H-1,2- oxathiole 2,2-dioxide and 3-alkyl-5H-4-amino-5-cyano-5H-2,3- dihydroisothiazole 1,1-dioxide in good yield. (C) 2000 Elsevier Science Ltd.
- Marco, José L.,Ingate, Simon T.,Jaime, Carlos,Beá, Ivan
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p. 2523 - 2531
(2007/10/03)
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- Regioselectivity of the photochemical addition of ammonia, phosphine, and silane to olefinic and acetylenic nitriles
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An investigation of the regioselectivity and mechanisms of the photochemical addition of NH3, PH3, and SiH4 to olefinic and acetylenic nitriles is described. The photolysis of NH3 in the presence of acrylonitrile led to the α-addition product 2-aminopropanenitrile (2), propanenitrile, and 2,3-dimethylbutanedinitrile (3). When NH3 was photolyzed in the presence of substituted derivatives (crotononitrile, methacrylonitrile, or 1-cyclohexenecarbonitrile), the α-addition products were still obtained. However, under similar reaction conditions, only the β-addition products, 7 and 8, were obtained from acrylonitrile and PH3, or acrylonitrile and SiH4, respectively. On the other hand, the photolysis of 2-butynenitrile and NH3 gave the β-addition products, (Z)- and (E)-3-aminocrotononitrile (10). The photolysis of these acetylenic nitriles with PH3 or SiH4 also gave the β-adducts (12) and (13). The α-addition of NH3 proceeds by the stepwise addition of H· and ·NH2, respectively, to the α,β-unsaturated nitriles. The β-addition products are formed by a radical chain mechanism initiated by photochemically generated radicals. The radical chain pathway provides an explanation for a number of previously described photochemical additions to olefins and acetylenes. Photochemical processes similar to the addition of ammonia and phosphine to unsaturated organic compounds may have played a role in the evolution of the atmosphere of the primitive Earth, and may even be currently occurring in the atmospheres of other planets.
- Guillemin, Jean-Claude,Breneman, Curt M.,Joseph, Jeffrey C.,Ferris, James P.
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p. 1074 - 1082
(2007/10/03)
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- Process for the preparation of an aminoitrile by partial hydrogenation of a nitrile compound with two or more nitrile groups
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The invention relates to a process for the preparation of an aminonitrile by partially hydrogenating a nitrile compound with two or more nitrile groups in the presence of a catalyst which contains a metal from group 8 of the periodic system of the elements, the hydrogenation being carried out under water-free reaction conditions and the catalyst having been treated with an alkanolate. Preferably, the catalyst is a Raney nickel or Raney cobalt catalyst which has been pretreated with an alkali metal alkanolate or an earth alkali metal alkanolate such as sodium or potassium methanolate.
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- SYNTHESE D'IMINES LINEAIRES NON-STABILISEES PAR REACTIONS GAZ-SOLIDE SOUS VIDE(1).
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Unstabilized imines are synthetized in gram-scale by vacuum dehydrochlorination of N-chloroalkylamines and by vacuum dehydrocyanation of α-aminonitriles on solid base.All the new compounds are characterized at low temperature by 1H, 13C NMR and IR spectroscopy.
- Guillemin, Jean-Claude,Denis, Jean-Marc
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p. 4431 - 4446
(2007/10/02)
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