反应详情

To a stirred solution of (3RS,4R)-2-methyl-4-(trityl-amino)-hexan-3-ol (0.53 g, 1 eq, 1.41 mmol) in DCM (20 mL) under an argon atmosphere at room temperature, was added CF3COOH (5 mL) dropwise, and the solution was stirred at this temperature for 1 h. The solvent was evaporated in vacuo, the residue was precipitated from Et2O (10 mL) with hexane (90 mL) with stirring to give a yellow oil. The solvent was decanted from the oil, and the oil was washed with hexane (20 mL) and dried in vacuo to afford the title compound as a light yellow oil. Yield: 0.18 g (100%). (50% de 3S,4R: 50% de 3R,4R). 1H-NMR (d6-DMSO, 250 MHz): δ 0.85-0.99 (m, 9H, NH2CH (CH2CH3)CH(CH(CH2)OH;, 1.42-1.79 (m, 2H, NH2CH(CH2CH3)CH (CH(CH3)2) OH), 2.95 (m, 1H, NH2CH(CH2CH3)CH(CH(CH3)2)OH), 3.18 (m, 1H, NH2CH (CH2CH3)CH(H(CH(CH3)2)OH), 3.37 (m, 1H, NH2CH(CH2CH3)CH(CH(CH3)2)OH, 7.58 (bs, 2H, NH2CH(CH2CH3)CH(CH(CH3)2)OH).

1. customThe solvent was evaporated in vacuo
2. customthe residue was precipitated from Et2O (10 mL) with hexane (90 mL)
3. stirringwith stirring
4. customto give a yellow oil
5. customThe solvent was decanted from the oil
6. washthe oil was washed with hexane (20 mL)
7. customdried in vacuo