Androstanol alkyl carbonic ether compound and preparation process thereof
A technology for androstanol alkyl carbonate and compound is applied in the field of organic compound and organic compound preparation, and can solve problems such as troublesome, uneconomical, low oral activity and the like
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example 2
[0018] 10g androstene corresponding compound 1-androstene-3β, 17β-diol was dissolved in 150g dichloromethane, N 2 Protect, electromagnetically stir, add 50g of triethylamine, slowly dropwise add 38g of methyl chloroformate corresponding to alkyl chloroformate, control the reaction temperature at 55-60°C, and stir for 5 hours. The reaction solution was washed 3 times with 10% hydrochloric acid, each hydrochloric acid consumption 15g; then washed with saturated NaCl aqueous solution (15g × 3), anhydrous NaCl 2 SO 4 Drying, removing the solvent under reduced pressure to obtain an oily crude product, the crude product was separated by silica gel column chromatography, the eluent was a mixture of petroleum ether and ethyl acetate, petroleum ether:ethyl acetate=10:1, and the product androstanol alkyl Carbonate corresponding compound 1-androstene-3β, 17β-diol bis(methyl carbonate) 13.47g, yield 96.2%. Example 2: One of the androstyl alkyl carbonate compounds 1-androstene-3β, 17β-di...
Embodiment 3
[0020] Except triethylamine consumption is 30g, methyl chloroformate consumption is 23g, all the other operations are with example 1, get 1-androstene-3β, 10.19g of 17β-diol bis(methyl carbonate) ester, yield 72.8%, simultaneously 1.20 g of a mixture of 1-androstene-3β, 17β-diol 3-(methyl carbonate) ester and 1-androstene-3β, 17β-diol 17-(methyl carbonate) ester were obtained. Example 3: 5α-androsterol-3β, 17β-diol bis
[0021] Preparation of (Benzyl Carbonate) Ester
[0022] 10g of the corresponding compound of androsterols 5α-androst-3β, 17β-diol was dissolved in 150g of dichloromethane, N 2 Protect, electromagnetically stir, add 50g of triethylamine, slowly dropwise add 68g of benzyl chloroformate corresponding compound of alkyl chloroformate, control the reaction temperature at 55-60°C, and stir for 5 hours. The reaction solution was washed 3 times with 10% hydrochloric acid, each hydrochloric acid consumption 15g; then washed with saturated NaCl aqueous solution (1...
Embodiment 4
[0022] 10g of the corresponding compound of androsterols 5α-androst-3β, 17β-diol was dissolved in 150g of dichloromethane, N 2 Protect, electromagnetically stir, add 50g of triethylamine, slowly dropwise add 68g of benzyl chloroformate corresponding compound of alkyl chloroformate, control the reaction temperature at 55-60°C, and stir for 5 hours. The reaction solution was washed 3 times with 10% hydrochloric acid, each hydrochloric acid consumption 15g; then washed with saturated NaCl aqueous solution (15g × 3), anhydrous NaCl 2 SO 4 Drying, removal of solvent under reduced pressure, the oily crude product was obtained, the crude product was separated by silica gel column chromatography, the eluent was a mixture of petroleum ether and ethyl acetate, petroleum ether:ethyl acetate=10:1, and the product androstanol alkyl Carbonate corresponding compound 5α-androst-3β, 17β-diol bis(benzyl carbonate) 17.64g, yield 92%. Example 4: 19-desmethylandrost-4-ene-3β, one of the androsty...
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