HRID653079

反应详情

EQUATION

反应方程式

HRID 653079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
89 °C

PROCEDURE

实验过程

1-[2-Hydroxy-3-propyl-4-(4-thiocyanomethylphenylmethoxy)phenyl]ethanone (6.0 g; 0.017 m) was dissolved in dioxan:water (80:20; 100 ml) to which was added sodium azide (4.4 g; 0.068 m) and ammonium chloride (1.8 g; 0.034 m). The resulting solution was heated at 89° C. for 18 hours, cooled and poured onto water. The resulting solution was acidified with concentrated hydrochloric acid, filtered and washed with water to leave a white solid. Recrystallised from methanol to give a cream crystalline solid m.p. 160°-161° C.

WORKUP

后处理

  1. temperaturecooled
  2. additionpoured onto water
  3. filtrationfiltered
  4. washwashed with water
  5. customto leave a white solid
  6. customRecrystallised from methanol