Invention Grant
- Patent Title: Preparation method for high purity racemic adrenaline
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Application No.: US16646506Application Date: 2019-03-05
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Publication No.: US10793512B2Publication Date: 2020-10-06
- Inventor: Yin Wang , Aoxiang Zhang , Yonggang Xu , Song Chen , Haoning Zhang
- Applicant: AMPHASTAR NANJING PHARMACEUTICALS INC.
- Applicant Address: CN Nanjing
- Assignee: AMPHASTAR NANJING PHARMACEUTICALS INC.
- Current Assignee: AMPHASTAR NANJING PHARMACEUTICALS INC.
- Current Assignee Address: CN Nanjing
- Agency: Reising Ethington, P.C.
- Priority: com.zzzhc.datahub.patent.etl.us.BibliographicData$PriorityClaim@77ac4e59
- International Application: PCT/CN2019/076945 WO 20190305
- International Announcement: WO2019/154436 WO 20190815
- Main IPC: C07C215/56
- IPC: C07C215/56

Abstract:
Disclosed is a preparation method for a racemic adrenaline as represented by formula II. The method comprises the following steps: compound 1 is directly racemized in an acidic solution to produce compound 2, the acid solution comprising neither sodium bisulfite nor salicylic acid; and specifically comprises (a), in the acid solution of which the pH is 0.5-1.5, compound 1 is placed under the protection of nitrogen gas and, with the reaction temperature being controlled at 75-95° C., stirred and reacted for 1-3 hours; (b) the reaction solution is controlled at a temperature of 5-20° C., into which an activated carbon is added, under the protection of nitrogen gas, stirred for 20-40 minutes, and filtered, then a filtrate is collected; the filtrate is controlled at a temperature of 5-20° C., the pH thereof is adjusted using ammonia to 8.5-9.5, and is filtered when the pH is stabilized, and a filter cake is washed and dried to produce a high purity racemic adrenaline white powder. The weight yield of the product produced per the preparation method of the present invention is greater than 90%, the chromatographic purity is greater than 96%, and the ee value approaches zero; the invention is inexpensive, simple to operate, favors industrialized production, and has a broad application prospect.
Public/Granted literature
- US20200270199A1 PREPARATION METHOD FOR HIGH PURITY RACEMIC ADRENALINE Public/Granted day:2020-08-27
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