HRID970631

反应详情

EQUATION

反应方程式

HRID 970631 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 6.72 g (45 mmol) of butylphenylamine in 50 ml of methylene chloride cooled to 10° C. was added slowly with stirring 6.67 g (22.5 mmol) of triphosgene in 40 ml of methylene chloride. The reaction was allowed to continue at room temperature for 27 hours. The solvent was evaporated and the residue extracted twice with n-hexane. The organic solution was concentrated in vacuo to yield 9.11 g (43.03 mmol) of a yellow oil (96%). 1H-NMR (CDCl3):δ 0,9 (m, 3H), 1,3 (m, 2H), 1,6 (m, 2H), 3,7 (m, 2H), 7,2–7,4 (m, 5H).

WORKUP

后处理

  1. additionwas added slowly
  2. customThe solvent was evaporated
  3. extractionthe residue extracted twice with n-hexane
  4. concentrationThe organic solution was concentrated in vacuo