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 (2 mL)-under an argon atmosphere at room temperature, was added trifluoroacetic acid (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 ether (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 (6-DMSO, 250 MHz): δ 0.85-0.99 (m, 9H, NH2CH(CH2CH3)CH(CH(CH3)2)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(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 ether (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