(3R,5S,8R,9S,10S,13R,14S,17R)-10,13-二甲基-17-[(2R)-6-甲基庚烷-2-基]-2,3,4,5,6,7,8,9,11,12,14,15,16,17-十四氢-1H-环戊烷[a]菲-3-胺

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2.04 g (4.83 mmol) 3α-azido-5α-cholestane in 50 ml THF, 16 ml (16 mmol) of a 1M solution of LiAlH4 in ether are carefully added dropwise. The mixture is heated for 4 h under reflow, cooled to RT, followed by cautious addition of 5 ml of a saturated NH4Cl solution. After filtration and washing of the residual filtrate twice with ether, the ether phase is dried over Na2SO4 and concentrated. The amine is obtained as white solid and directly processed further. Yield 96%, F=95-97° C. C27H49N (387.7), calc. C, 83.65; H, 12.74; N, 3.61. found: C, 83.30; H, 12.42; N, 3.65. The mixture is heated for 4 h under reflow After filtration washing of the residual filtrate twice with ether the ether phase is dried over Na2SO4 concentrated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2.04 g (4.83 mmol) 3α-azido-5α-cholestane in 50 ml THF, 16 ml (16 mmol) of a 1M solution of LiAlH4 in ether are carefully added dropwise. The mixture is heated for 4 h under reflow, cooled to RT, followed by cautious addition of 5 ml of a saturated NH4Cl solution. After filtration and washing of the residual filtrate twice with ether, the ether phase is dried over Na2SO4 and concentrated. The amine is obtained as white solid and directly processed further. Yield 96%, F=95-97° C. C27H49N (387.7), calc. C, 83.65; H, 12.74; N, 3.61. found: C, 83.30; H, 12.42; N, 3.65. The mixture is heated for 4 h under reflow After filtration washing of the residual filtrate twice with ether the ether phase is dried over Na2SO4 concentrated