HRID1819480
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
To a solution of (4-pyrrolidin-1-yl-cyclohexylmethyl)-carbamic acid benzyl ester (292 mg, 0.92 mmol) in MeOH (5 mL) was added ammonium formate (0.58 g, 9.20 mmol). The reaction flask was flushed with N2 prior to addition of 10% Pd/C (300 mg). The mixture was heated at 65° C. for 2 h whereupon TLC analysis (silica gel, 95:4.75:0.25 DCM/MeOH/NH4OH) showed complete consumption of 57. After cooling to room temperature the reaction mixture was filtered through a plug of celite in order to remove the Pd catalyst. The filtrate contained (4-pyrrolidin-1-yl-cyclohexyl)-methylamine which was used without further purification in the next step.
WORKUP
后处理
- customThe reaction flask was flushed with N2
- additionto addition of 10% Pd/C (300 mg)
- customconsumption of 57
- temperatureAfter cooling to room temperature the reaction mixture
- filtrationwas filtered through a plug of celite in order
- customto remove the Pd catalyst
- customwas used without further purification in the next step