New organic compound 4-androstene-3beta, 17 beta-diol bis (ethylcarbonyldioxy) ester and its prepn
A technology of organic compounds and androstene, which is applied in the field of new organic compounds and organic compound preparations, can solve the problems of low oral activity, liver danger, trouble, etc., and achieve the effect of high yield, good oral activity, and simple preparation process
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Embodiment 1
[0015] Example 1. Dissolve 10g of 4-androstenediol in 150g of dichloromethane, N 2 protection, electromagnetic stirring, adding 50 g of triethylamine, slowly dropwise adding 40 g of ethyl chloroformate, controlling the reaction temperature at 50-60° C., and reacting for 5 hours. The reaction solution was washed 3 times with 15 g of 10% hydrochloric acid, 3 times with 15 g of saturated NaCl aqueous solution, anhydrous NaCl 2 SO 4 Dry, and remove the solvent under reduced pressure to obtain a crude product, which is separated by silica gel column chromatography, and the eluent is a mixed solution of petroleum ether and ethyl acetate, petroleum ether:ethyl acetate=10:1, and the product 4-androstene- 3β, 17β-diol bis(ethyl carbonate) 14.4g, yield 96%. m.p.110-112°C.
Embodiment 2
[0016] Example 2. Dissolve 10g of 4-androstenediol in 150g of dichloromethane, N 2 protection, electromagnetic stirring, adding 40 g of triethylamine, slowly adding 30 g of ethyl chloroformate, controlling the reaction temperature at 50-60° C., and reacting for 5 hours. The reaction solution was washed 3 times with 15 g of 10% hydrochloric acid, 3 times with 15 g of saturated NaCl aqueous solution, anhydrous NaCl 2 SO 4 Dry, and remove the solvent under reduced pressure to obtain the crude product, which is separated by silica gel column chromatography, and the eluent is a mixed solution of petroleum ether and ethyl acetate, petroleum ether:ethyl acetate=10:1, to obtain a white crystalline powder 4- Androstene-3β, 17β-diol bis(ethyl carbonate) 13.0 g, yield 86.7%. m.p.110-113°C.
Embodiment 3
[0017] Example 3. Dissolve 10g of 4-androstenediol in 150g of dichloromethane, N 2 protection, electromagnetic stirring, adding 30 g of triethylamine, slowly adding 20 g of ethyl chloroformate, controlling the reaction temperature at 50-60° C., and reacting for 5 hours. The reaction solution was washed 3 times with 15 g of 10% hydrochloric acid, 3 times with 15 g of saturated NaCl aqueous solution, anhydrous NaCl 2 SO 4 Dry, and remove the solvent under reduced pressure to obtain the crude product, which is separated by silica gel column chromatography, and the eluent is a mixed solution of petroleum ether and ethyl acetate, petroleum ether:ethyl acetate=10:1, to obtain a white crystalline powder 4- Androstene-3β, 17β-diol bis(ethyl carbonate) 12.0 g, yield 80%. m.p.111.5~113.5℃.
[0018] The present invention is particularly suitable for preparing novel organic compound 4-androstene-3β, 17β-diol bis(ethyl carbonate). The new organic compound has good oral activity and is...
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