反应详情

To a solution of (R)-methyl 2-amino-2-(5-bromo-2-fluorophenyl)propanoate (3.95 g, 14.3 mmol, Eq: 1.00) in diethyl ether (120 ml) was added at 0° C. lithium aluminum hydride (652 mg, 17.2 mmol, Eq: 1.2) in five portions. The icebath was removed and stirring continued at room temperature for 2 hours. To the cooled reaction mixture was added dropwise water (652 mg, 652 μl, 36.2 mmol, Eq: 2.53), NaOH (15% in water) (572 mg, 652 μl, 14.3 mmol, Eq: 1.00) and water (1.96 g, 1956 μl, 109 mmol, Eq: 7.59) via syringe (1:1:3 system) and the mixture was stirred for 20 min until a white suspension occurred. Three small spoons of Na2SO4 were added to the mixture, which was filtered after 5 min. The colourless ether solution was evaporated to give (R)-2-amino-2-(5-bromo-2-fluorophenyl)propan-1-ol (3.2 g, 12.9 mmol, 90.2% yield) as a white solid which was used in the next step without further purification. MS (ISP): m/z=248.1 [M+H]+ and 250.0 [M+2+H]+.

1. customThe icebath was removed
2. customTo the cooled reaction mixture
3. stirringthe mixture was stirred for 20 min until a white suspension
4. filtrationwas filtered after 5 min
5. customThe colourless ether solution was evaporated