反应详情

温度

0 °C

A solution of methyl 2-(2-(piperidin-1-yl)ethylamino)-3-fluorobenzoate (740 mg, 2.640 mmol) in Et2O (30 mL) at −20° C. was treated with LAH (128 mg, 3.372 mmol). After 1.5 hours additional LAH (20 mg, 0.5269 mmol) was added and the reaction was warmed to 0° C. At 0° C., the reaction was diluted with Et2O (80 mL), then NaF and water were added with vigorous stirring until a white ppt formed and the solution cleared. The solution was decanted and evaporated under vacuum. The crude material was purified on a 12 g Redisep ISCO column with 0-10% MeOH in CH2Cl2 over 40 CV to yield (2-(2-(piperidin-1-yl)ethylamino)-3-fluorophenyl)methanol (453 mg, 179.5 mmol) as an off-white solid. FIA: 253.19 (M+1).

1. customformed
2. customThe solution was decanted
3. customevaporated under vacuum
4. customThe crude material was purified on a 12 g Redisep ISCO column with 0-10% MeOH in CH2Cl2 over 40 CV