HRID1834411
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was warmed
- dissolutionto dissolve this,
- customThe product was separated
- washwashed with dilute hydrochloric acid
- customIt formed colourless micro-prisms (549 mg. 77%), m.p. 166°-167° C. or 173-174.5° C.
- customafter changing to cubes at about 136° C
- customFor analysis it was recrystallized from aqueous ethanol as prismatic rods, m.p. 172° C.