Ethisterone synthesis
- Product Name:Ethisterone
- CAS Number:434-03-7
- Molecular formula:C21H28O2
- Molecular Weight:312.45
Yield:434-03-7 109.3 g
Reaction Conditions:
Stage #1:acetylene with potassium hydroxide in tetrahydrofuran;ethanol at 3; for 2 h;Inert atmosphere;
Stage #2:Androstenedione in tetrahydrofuran;ethanol for 2 h;Temperature;Solvent;Reagent/catalyst;
Steps:
1.1 The first step, acetylation reaction:
In a dry three-necked flask, potassium hydroxide (200 g, 2W), Tetrahydrofuran (1000 ml, 10 V) and ethanol (120 ml, 1.2 V),Heated to 50 ° C under nitrogen for 1 hour, cooled to 3 ° C,Acetylene gas was passed at this temperature for 2 hours.Preparation of 4-androstenedione (I) in tetrahydrofuran solution:4-androstenedione (I) (100 g, 1 W) was dissolved in tetrahydrofuran(200ml, 2V), the solution was slowly added dropwise, incubated for 2 hours.With 10% aqueous hydrochloric acid to adjust the pH to 3 ~ 4,Heated to reflux for half an hour, the solvent was removed under reduced pressure,Water (1000ml, 10V) was added to the solution, and the mixture was filtered, washed with water,The mixture was dried under reduced pressure at 60 ° C to give the acetylide II (109.3 g) in a weight yield of 109% and an HPLC content of 96%.
References:
Zhejiang Xianju Pharmaceutical Co., Ltd.;Chen Dejia;Dai Jing;Fang Weiming CN106317154, 2017, A Location in patent:Paragraph 0028; 0030
3604-60-2
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