- Synthesis method of atropine and atropine sulfate
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The invention provides a synthesis method of atropine and atropine sulfate, which comprises the following steps: carrying out acetylation reaction on tropine acid to form acetyl tropine acid, reactingthe acetyl tropine acid with a chlorination reagent to form acyl chloride, reacting the acyl chloride with tropine alcohol, removing acetyl to obtain atropine, and salifying atropine and sulfuric acid to obtain atropine sulfate. The whole synthesis process can be completed by adopting a one-pot reaction, additional steps for completing the process by isolating intermediates are avoided, the reaction conditions are mild, the steps are simple, the yield is high, the purity is high, and the method is suitable for large-scale industrial production.
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Paragraph 0042-0044; 0066-0068
(2020/07/02)
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- N- Ethylpyridine methylamine hydrochloride and crystal, preparation process and application thereof
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The invention discloses N -ethyl-pyridine methylamine trifluoroacetate, and a crystal. preparation process and application N - thereof to prepare N -ethylpyridine methylamine hydrochloride crystals, by slowly adding X -ethyl-pyridine methylamine, in an organic solvent 15.12 °, 15.45 °, 17.68 °, 20.68 °, 22.62 °, 23.25 °, 24.75 °, 29.54 ° at room temperature or heating. to fully dissolve N -ethyl-pyridine methylamine . through heating for, hours to prepare the ethyl-pyridine methylamine trifluoroacetate crystals . The method is simple in operation and;% in crystal form impurity content, obtained by dry-adding trifluoroacetic acid; crystals, at about, at room temperature or, in a heating mode of heating the crystals at a temperature ranging from, N - degrees, to a. material completely-dissolving solution.
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Paragraph 0052-0057
(2020/03/17)
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- N-ethylpyridine methylamine mesylate crystal, preparation process thereof and application of N-ethylpyridine methylamine mesylate crystal in preparation of tropicamide
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The invention discloses an N-ethylpyridine methylamine mesylate crystal, a preparation process thereof and the application of the N-ethylpyridine methylamine mesylate crystal in the preparation of tropicamide. Mesylate of N-ethylpyridine methylamine mesylate crystal is prepared from N-ethylpyridine methylamine and methylsulfonic acid, when X-ray powder diffraction is used, and the crystal has diffraction peaks at about 9.49 degrees, 13.16 degrees, 16.18 degrees, 19.10 degrees, 20.54 degrees, 23.24 degrees, 26.96 degrees and 34.63 degrees. The preparation method comprises the following steps ofdissolving the N-ethylpyridine methylamine in an organic solvent, and stirring at room temperature or heating and stirring until a material is completely dissolved; slowly adding acid, and crystallizing; and carrying out heat preservation aging, filtering and drying to obtain the tropicamide key starting material N-ethylpyridine methylamine mesylate crystal. The method is simple to operate and obvious in purification effect, the salt form impurity content and the crystal form impurity content prepared by crystallization are low, the purity is high, and the industrial production is facilitated.
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Paragraph 0024; 0025
(2020/04/17)
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- Construction of 8-Azabicyclo[3.2.1]octanes via Sequential DDQ-Mediated Oxidative Mannich Reactions of N-Aryl Pyrrolidines
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A concise synthesis of 8-azabicyclo[3.2.1]octanes via sequential oxidative Mannich reactions is described. This approach involves an intermolecular oxidative Mannich coupling reaction between N-aryl pyrrolidines with TMS enol ether and a subsequent intramolecular oxidative Mannich cyclization of the corresponding silyl enol ether. DDQ is used as a key oxidant for both reactions.
- Jo, Hanbyeol,Hassan, Ahmed H. E.,Jung, Seung Young,Lee, Jae Kyun,Cho, Yong Seo,Min, Sun-Joon
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supporting information
p. 1175 - 1178
(2018/02/23)
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- PhSO2SCF2H: A Shelf-Stable, Easily Scalable Reagent for Radical Difluoromethylthiolation
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A new shelf-stable and easily scalable difluoromethylthiolating reagent S-(difluoromethyl) benzenesulfonothioate (PhSO2SCF2H) was developed. PhSO2SCF2H is a powerful reagent for radical difluoromethylthiolation of aryl and alkyl boronic acids, decarboxylative difluoromethylthiolation of aliphatic acids, and a phenylsulfonyl-difluoromethylthio difunctionalization of alkenes under mild reaction conditions.
- Zhu, Dianhu,Shao, Xinxin,Hong, Xin,Lu, Long,Shen, Qilong
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supporting information
p. 15807 - 15811
(2016/12/16)
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- Gold(I)/copper(II)-cocatalyzed tandem cyclization/semipinacol reaction: Construction of 6-Aza/Oxa-Spiro[4.5]decane skeletons and formal synthesis of (±)-halichlorine
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A simple and efficient strategy for the construction of 6-aza/oxa-spiro[4.5]decane skeletons under the cocatalysis of gold(I)/copper(II) was developed, and its potential utility was demonstrated by a formal synthesis of the biologically active marine alkaloid (±)-halichlorine.
- Zhu, Dao-Yong,Zhang, Zhen,Mou, Xue-Qing,Tu, Yong-Qiang,Zhang, Fu-Min,Peng, Jin-Bao,Wang, Shao-Hua,Zhang, Shu-Yu
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supporting information
p. 747 - 752
(2015/03/18)
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- Markedly enhancing enzymatic enantioselectivity in organic solvents by forming substrate salts
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A new approach is proposed to enhance enzymatic enantioselectivity in organic solvents. It is based on the presumption that the less reactive substrate enantiomer experiences greater steric hindrances in the enzyme- bound transition state than the more re
- Ke, Tao,Klibanov, Alexander M.
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p. 3334 - 3340
(2007/10/03)
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- Differential analgesic activity of the enantiomers of atropine derivatives does not correlate with their muscarinic subtype selectivity
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The enantiomers of several tropic and p-substituted tropic acid esters related to atropine obtained by esterification under non-racemizing conditions after resolution of the corresponding racemic acids [(+)- and (-)-18, (+)- and (-)-19] are reported. They were tested in vitro on muscarinic subtype receptors and in vivo for their analgesic activity on mice. As in the case of the lead compound, R-(+)-hyoscyamine, these substances show enantioselectivity in analgesic tests, the eutomers being the R-(+) or R-(+)-p-substituted tropic acid derivatives. However, this property, which is a consequence of increased central release of ACh, seems unrelated to muscarinic subtype selectivity insofar as the compounds are unable to discriminate muscarinic subtype receptors. A possible explanation of these results which does not involve subtype selectivity is proposed, based on the recently developed concept of inverse agonism.
- Dei,Bartolini,Bellucci,Ghelardini,Gualtieri,Manetti,Romanelli,Scapecchi,Teodori
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p. 595 - 605
(2007/10/03)
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- Synthesis, characterization and pharmacological profile of tropicamide enantiomers
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The synthesis, chemical characterization and antimuscarinic activity of the two enantiomers of tropicamide are reported. Functional (rabbit vas deferens, guinea pig heart (force) and ileum) as well as binding experiments (m1 and m4 human muscarinic receptors expressed in CHO-K1 cells; M2 and M3 receptors of rat heart and submaxillary gland membranes) were used to evaluate the antimuscarinic activity of the enantiomers. The results show that none of the enantiomers is able to significantly discriminate among the receptors studied and therefore do not support the proposal of tropicamide as an M4 (m4) selective agent.
- Dei, Silvia,Bellucci, Cristina,Ghelardini, Carla,Romanelli, M. Novella,Spampinato, Santi
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p. 2147 - 2153
(2007/10/03)
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- Analgesic, antimuscarinic activity and enantioselectivity of the four isomers of 3-quinuclidinyl tropate as compared with the enantiomers of hyoscyamine
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The four stereoisomers of 3-quinuclidinyl tropate (2) were synthesized and their absolute configuration established. The analgesic activity of the four isomers on the hot-plate test and their muscarinic antagonism on rabbit vas deferens (M1), g
- Dei,Bellucci,Gualtieri,Romanelli,Scapecchi,Teodori,Bartolini,Ghelardini
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p. 303 - 309
(2007/10/02)
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- Enzymatic preparation of optically active fungicide intermediates in aqueous and in organic media
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Pure stereoisomers of two new triazole and morpholine fungicides have been prepared starting from enzymatically synthesized chiral alcohol intermediates.Two resolution strategies compared are: lipase-catalyzed hydrolysis of corresponding acetates in water and lipase-catalyzed transesterification of alcohols in organic solvents.The antifungal activity of optically pure enantiomers of the synthesized fungicides investigated in vitro and in vivo against a variety of fungi, show an activity ratio (R-form/S-form) up to 400.
- Bianchi, Daniele,Cesti, Pietro,Golini, Paolo,Spezia, Sandro,Garavaglia, Carlo,Mirenna, Luigi
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p. 176 - 180
(2007/10/02)
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- Phenyl alpha acyloxyalkanoic acids, derivatives and their therapeutic use
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Therapeutic as well as preventative measures to improve the cosmetic conditions or to alleviate the symptoms of dermatologic disorders with phenyl alpha acyloxyalkanoic acids and derivatives is disclosed. The cosmetic conditions and dermatologic disorders
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