浙江化工2024,Vol.55Issue(1) :15-20.DOI:10.3969/j.issn.1006-4184.2024.01.003

16α-羟基泼尼松龙的合成工艺改进

Improvement for the Synthesis Process of 16α-Hydroxprednisolone

尹琳琳 王乐晓 陈益俊 金旦妮
浙江化工2024,Vol.55Issue(1) :15-20.DOI:10.3969/j.issn.1006-4184.2024.01.003

16α-羟基泼尼松龙的合成工艺改进

Improvement for the Synthesis Process of 16α-Hydroxprednisolone

尹琳琳 1王乐晓 1陈益俊 1金旦妮1
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作者信息

  • 1. 台州仙琚药业有限公司, 浙江 台州 317016
  • 折叠

摘要

针对原 16α-羟基泼尼松龙合成工艺原料成本高、消除反应选择性差等问题,开发了一种改进工艺.以 21-羟基孕甾-1,4,9(11),16-四烯-3,20-二酮-21-醋酸酯为原料,经氧化、溴羟化、脱溴及水解等 4 步反应合成目标化合物 16α-羟基泼尼松龙,降低了生产成本及三废排放量,并使反应总收率达到 82.2%.产物结构经 1H NMR、13C NMR和MS(ESI)等数据确证.改进后的合成工艺具有反应选择性好、成本低、总收率高等优点.

Abstract

In view of the problem of high raw material cost and poor selectivity in elimination reaction of the original 16α-hydroxyprednisolone synthesis process,an improved process was developed.The target product 16α-hydroxyprednisolone was synthesized from 21-hydroxypregna-1,4,9(11),16-tetraene-3,20-dione-21-acetate by oxidation,hydroxybromination,debromination and hydrolysis.The production cost and waste emissions were reduced,and the total yield of the reaction reached 82.2%.The structure of product was confirmed by 1H NMR,13C NMR and MS(ESI).The improved synthetic process has the advantages of good selectivity,low cost and high total yield.

关键词

16α-羟基泼尼松龙/21-羟基孕甾-1,4,9(11),16-四烯-3,20-二酮-21-醋酸酯/氧化反应/溴羟化反应/工艺改进

Key words

16α-hydroxprednisolone/21-hydroxypregna-1,4,9(11),16-tetraene-3,20-dione-21-acetate/oxidation/hydroxybromination/process improvement

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出版年

2024
浙江化工
浙江省化工研究院有限公司

浙江化工

影响因子:0.131
ISSN:1006-4184
参考文献量2
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