A kind of preparation method of 16-ene steroid compound
A technology of steroidal compounds and compounds, which is applied in the production of steroidal compounds, organic chemistry, bulk chemicals, etc., can solve the problems of miscellaneous products, inability to react, low yield, etc.
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Embodiment 1
[0048]
Embodiment 1-1
[0050]Compound 1 (5 g, 13.5 mmol) was dissolved in acetonitrile (100 ml), trimethylsilyl iodide (5.8 ml, 40.5 mmol) was added, the reaction was stirred at 50°C, and the reaction progress was monitored by TLC until the reaction was complete, and Na 2 S 2 O 3 After aq (300ml, 10%w / v) terminated the reaction, the liquid was separated, 200ml of ethyl acetate was extracted and separated, the combined organic phases were distilled under reduced pressure and recrystallized from ethyl acetate / petroleum ether to obtain a white solid 2 (4.4g), The purity is 98.5%, and the molar yield is 92%. After testing, a small amount of substance 2-1 is formed in the mother liquor.
Embodiment 1-2
[0052] Compound 1 (5g, 13.5mmol) was dissolved in acetonitrile (100ml), trimethylsilyl iodide (3.8ml, 27.0mmol) was added, the reaction was stirred at 50°C, and the reaction progress was monitored by TLC until the reaction was complete, and Na 2 S 2 O 3 After aq (300ml, 10%w / v) to terminate the reaction, 200ml of ethyl acetate was added to extract and separate the liquids. After distillation under reduced pressure, recrystallization from ethyl acetate / petroleum ether gave a white solid 2-1 (4.4g) with a purity of 99.2% , the molar yield was 92%, and after testing, a small amount of substance 2 was generated in the mother liquor.
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