HRID1709292

反应详情

EQUATION

反应方程式

HRID 1709292 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice cold solution of 5.5 g. (33 mmole) 4-(2-hydroxyethyl)-phenethylamine, 100 ml. methylene chloride and 3.4 g. (33 mmole) triethylamine is slowly added dropwise a solution of 7.2 g. (33 mmole) 4-azidobenzenesulphonyl chloride in 50 ml. methylene chloride. Subsequently, the reaction is allowed to continue for 1 hour with ice cooling. The reaction mixture is now shaken out twice with dilute sulphuric acid, then twice with water, dried with anhydrous sodium sulphate and finally evaporated. The residue is recrystallised twice from toluene to give 7.8 g. (64% of theory) of desired product; m.p. 90°-92° C. (recrystallised from toluene).

WORKUP

后处理

  1. dry with materialtwice with water, dried with anhydrous sodium sulphate
  2. customfinally evaporated
  3. customThe residue is recrystallised twice from toluene
  4. customto give 7.8 g