HRID46618

反应详情

EQUATION

反应方程式

HRID 46618 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a solution of 60.0 g (0.25 mol) of sodium sulfide nonahydrate in 500 ml of dimethyl formamide was gradually added 29 g (0.25 mol) of chloropyrazine in 100 ml of dimethyl formamide. The solution was stirred overnight at approximately 40° C. following which 52.5 g (0.25 mol) of 2-bromo-5-nitrothiazole was added as a solid. This reaction mixture was stirred at room temperature for 4 hours. After this period it was poured into water. The resulting precipitate was collected by suction filtration, washed with water and dried. The crude product was crystallized from methanol to yield 38 g (72% yield) of yellowish-gold crystals, m.p. 129°-130° C. A sample was subjected to elemental analysis. The results obtained were as follows:

WORKUP

后处理

  1. additionwas added as a solid
  2. stirringThis reaction mixture was stirred at room temperature for 4 hours
  3. filtrationThe resulting precipitate was collected by suction filtration
  4. washwashed with water
  5. customdried
  6. customThe crude product was crystallized from methanol
  7. customto yield 38 g (72% yield) of yellowish-gold crystals, m.p. 129°-130° C
  8. customThe results obtained