HRID1295872

反应详情

EQUATION

反应方程式

HRID 1295872 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of chlorodiphenylmethane (0.79 g, 3.22 mmol) in butanone (20 ml) was added methyl-pyrrolidine-3-ylmethyl-amine)-carbamic acid tert-butyl ester (0.69 g, 3.22 mmol), K2CO3 (0.54 g, 3.8 mmol) and KI (0.54 g, 3.22 mmol). The mixture was heated under reflux for 18 hours, then filtered and the solvent was removed in vacuo. The residue was dissolved in CH2Cl2 (50 ml) and washed with water (10 ml). Drying over MgSO4 and removal of solvent under reduced pressure followed by column chromatography using CH2Cl2:CH3OH (20:1) gives the desired product in 75% yield.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 18 hours
  3. filtrationfiltered
  4. customthe solvent was removed in vacuo
  5. dissolutionThe residue was dissolved in CH2Cl2 (50 ml)
  6. washwashed with water (10 ml)
  7. dry with materialDrying over MgSO4 and removal of solvent under reduced pressure