HRID1449429

反应详情

EQUATION

反应方程式

HRID 1449429 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Aminoethanol (1.2 g, 19.7 mmol) in dry dichloromethane (5 ml) was added dropwise to a solution of 9-fluorenylmethylchloroformate (5.0 g, 19.3 mmol) together with pyridine (1.5 g, 19.4 mmol). The mixture was stirred for a total of 1.25 hours then diluted with dichloromethane (50 ml), washed with water (25 ml), a saturated solution of ammonium chloride (25 ml), the organic phase was separated dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated in vacuo to give a white solid. This material was crystallised from dichloromethane to give 2-(9-fluorenylmethoxycarbonyl)aminoethanol.

WORKUP

后处理

  1. washwashed with water (25 ml)
  2. customa saturated solution of ammonium chloride (25 ml), the organic phase was separated
  3. dry with materialdried over anhydrous magnesium sulphate
  4. filtrationfiltered
  5. customthe filtrate evaporated in vacuo
  6. customto give a white solid
  7. customThis material was crystallised from dichloromethane