HRID1900083

反应详情

EQUATION

反应方程式

HRID 1900083 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.28 g (20 mmol) of 4-adamantan-1-yl-phenylamine hydrochloride were placed in 100 ml of methylene chloride and treated with 3.22 g (42.0 mmol) of pyridine. A solution of 2.39 g (22.0 mmol) of ethyl chloroformate in 15 ml of methylene chloride was added dropwise to this suspension at room temperature while stirring during 15 minutes. The reaction mixture was stirred at room temperature for 2 hours. Subsequently, the mixture was washed with water and the organic phase was dried over sodium sulfate, filtered and evaporated. The residue was recrystallized from methylene chloride/n-hexane. 5.6 g of ethyl 4-adamantan-1-yl-phenyl-carbamate were obtained as a white crystallizate. M.p.: 132°-134°.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at room temperature for 2 hours
  2. washSubsequently, the mixture was washed with water
  3. dry with materialthe organic phase was dried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was recrystallized from methylene chloride/n-hexane