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ChemicalBook CAS DataBase List Halcinonide

Halcinonide synthesis

3synthesis methods
-

Yield:3093-35-4 97.5%

Reaction Conditions:

with sulfur dioxide;propionyl chloride;diethylamine in chloroform at -10; for 1.5 h;

Steps:

4 present invention example 4
Compound 7 (7.0 g) was dissolved in chloroform (100 ml), cooled to -10 ° C, propionyl chloride (3.0 ml) was added, diethylamine (15 ml) was added, and SO2 (15% by weight to diethylamine) was added. After the reaction for 1.5 hours, the reaction solution was diluted to 500 ml of 0 ° C water, stirred for 2 hours, and the organic phase was separated by distillation under reduced pressure. Compound 8 (7.1 g, molar yield 97.5%, purity 98.9%) was obtained.

References:

Tianjin Pharmaceutical Institute Co., Ltd.;Li Yaling;Sun Jianlei CN109206466, 2019, A Location in patent:Paragraph 0057-0059

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