70110-25-7Relevant articles and documents
Preparation method of D-2-chloropropionyl chloride and D-2-chloropropionyl chloride
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Paragraph 0055; 0060-0065; 0070-0076; 0081-0086; 0101-0114, (2021/03/13)
The invention is applicable to the technical field of synthesis of medical intermediates, and provides a preparation method of D-2-chloropropionyl chloride and D-2-chloropropionyl chloride, the preparation method comprises the following steps: adding L-ethyl lactate and a catalyst into a reaction vessel, dropwisely adding thionyl chloride at -10-10 DEG C, heating to 65-70 DEG C, and carrying out heat preservation reaction; after the reaction is finished, cooling to 10-30 DEG C, and carrying out reduced pressure concentration and other treatment to obtain ethyl D-2-chloropropionate; adding resin, anhydrous formic acid and water, heating to 70-100 DEG C, and reacting for 2-5 hours; after the reaction is finished, cooling to 10-30 DEG C, filtering, and distilling to obtain D-2-chloropropionicacid; and dropwise adding thionyl chloride at 0-5 DEG C, heating to 45-65 DEG C, carrying out heat preservation reaction, and carrying out vacuum concentration and distillation treatment to obtain the product. The method realizes 10kg-grade large-scale production of D-2-chloropropionyl chloride, and has the advantages of high yield, high purity, recyclable catalyst, and no need of rectification equipment.
Production process of chloropropionyl glutamine
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Paragraph 0023-0026; 0030-0033; 0035, (2020/03/09)
The invention relates to the technical field of chemical engineering, and discloses a production process of chloropropionyl glutamine. The production process comprises following steps: carrying out acylating chlorination reaction: adopting D-2-chloropropionic acid and thionyl chloride as raw materials, adopting DMF (N, N-dimethylformamide) as a catalyst, and carrying out reaction to generate D-2-chloropropionyl chloride, sulfur dioxide and hydrogen chloride. According to the production process of chloropropionyl glutamine, 791kg of thionyl chloride is pressed into a dry and clean 2000 L enamelreaction kettle by using nitrogen, stirring is started, and 0.75kg of N, N-dimethylformamide is slowly dropwise added; then, 600kg of D-2-chloropropionic acid is pressed into a dry and clean 1000L enamel high-level tank by using nitrogen gas, a reaction kettle jacket is subjected to 75 DEG C hot water bath to increase the temperature of the system to 60-65 DEG C, D-2-chloropropionic acid is dropwise added into the reaction kettle for about 4 h at 60 to 65 DEG C, and the gas release amount is controlled by adjusting the dropwise adding speed. T production process is simple in steps, complete in reactant reaction, high in raw material utilization rate and low in preparation cost, troubles of users are avoided, and the production process is convenient for users to use.
PROCESS FOR PREPARING 7H-PYRROLO[2,3-d]PYRIMIDINE DERIVATIVES AND SYNTHETIC INTERMEDIATES THEREOF
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Paragraph 0405-0407; 0444; 0445; 0622-0626; 0632-0634, (2020/07/23)
The present invention provides processes for preparing 7H-pyrrolo[2,3-d]pyrimidine derivatives, which are useful as a Janus kinase (JAK) inhibitor, intermediates thereof, and processes for preparing the intermediates. The present invention provides processes for preparing 3-[(3S, 4R)-3-methyl-6-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1,6-diazaspiro[3.4]octan-1-yl]-3-oxopropanenitrile using salts of (3S,4R)-1-benzyl-3-methyl-1,6-diazaspiro[3.4]octane with organic acids.