HRID981097
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
17.3 g (58 mmol) of crude trans-1-benzyl-3-benzylmethylamino-4-hydroxy-pyrrolidine in 80 ml of absolute tetrahydrofuran are added dropwise to 2.8 g (93.3 mmol) of 80% strength sodium hydride in 40 ml of absolute tetrahydrofuran and the mixture is heated under reflux at the same time. When the evolution of hydrogen has ended, 8.7 g (61 mmol) of methyl iodide are added dropwise and the mixture is then heated under reflux overnight. It is poured into ice-water and extracted with toluene, the extracts are dried with K2CO3, and concentrated and the residue is distilled.
WORKUP
后处理
- temperaturethe mixture is heated
- temperatureunder reflux at the same time
- temperaturethe mixture is then heated
- temperatureunder reflux overnight
- extractionextracted with toluene
- dry with materialthe extracts are dried with K2CO3
- concentrationconcentrated
- distillationthe residue is distilled