HRID1834411

反应详情

EQUATION

反应方程式

HRID 1834411 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

Anhydrous stannous bromide (5g) was stirred to solution in 20 ml of hydrogen bromide in acetic acid (30-32 %). 2,4-Dimethyl-3-acetyl-pyrrole (548 mg) was added and the mixture was warmed to dissolve this, then cooled to 30° C. Acetone(0.6 ml) was added and the solution was stirred at 35° C. for 21/2 hrs then poured into water at 10° C. The product was separated and washed with dilute hydrochloric acid then with water. It formed colourless micro-prisms (549 mg. 77%), m.p. 166°-167° C. or 173-174.5° C. after changing to cubes at about 136° C. For analysis it was recrystallized from aqueous ethanol as prismatic rods, m.p. 172° C.

WORKUP

后处理

  1. temperaturethe mixture was warmed
  2. dissolutionto dissolve this,
  3. customThe product was separated
  4. washwashed with dilute hydrochloric acid
  5. customIt formed colourless micro-prisms (549 mg. 77%), m.p. 166°-167° C. or 173-174.5° C.
  6. customafter changing to cubes at about 136° C
  7. customFor analysis it was recrystallized from aqueous ethanol as prismatic rods, m.p. 172° C.