反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of [(S)-1-(7-methyl-1-phenyl-1H-benzoimidazol-2-yl)ethyl]carbamic acid benzyl ester (1.5 g, 3.89 mmol) and 10% Pd/C (150 mg) in IMS (25 mL) was degassed with a stream of nitrogen and, after addition of HCl (1M, 2.5 mL), was stirred at RT (room temperature) under a hydrogen atmosphere for 5.5 h. The suspension was then filtered through a pad of Celite® and the filtrate was concentrated in vacuo. The resulting residue was partitioned between DCM (dichloromethane) and water, the organic layer was then washed with a saturated solution of NaHCO3, dried (Na2SO4) and concentrated in vacuo affording (S)-1-(7-Methyl-1-phenyl-1H-benzoimidazol-2-yl)ethylamine as a brown solid (1.41 g, 96%). LCMS: RT 2.07 min [M−NH2]1 235.1
WORKUP
后处理
- customwas degassed with a stream of nitrogen
- additionafter addition of HCl (1M, 2.5 mL)
- filtrationThe suspension was then filtered through a pad of Celite®
- concentrationthe filtrate was concentrated in vacuo
- customThe resulting residue was partitioned between DCM (dichloromethane) and water
- washthe organic layer was then washed with a saturated solution of NaHCO3
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo