反应 #74896

反应方程式

water

sodium sulfide nonahydrate

chloropyrazine

2-bromo-5-nitrothiazole

→

((5-nitro-2-thiazolyl)thio)Pyrazine

收率 72.0%

溶剂

dimethyl formamide

dimethyl formamide

反应条件

后处理

1. 1
   workup.ADDITIONwas added as a solid
2. 2
   workup.STIRRINGThis reaction mixture was stirred at room temperature for 4 hours
3. 3
   过滤The resulting precipitate was collected by suction filtration
4. 4
   洗涤washed with water
5. 5
   其他dried
6. 6
   其他The crude product was crystallized from methanol
7. 7
   其他to yield 38 g (72% yield) of yellowish-gold crystals, m.p. 129°-130° C
8. 8
   其他The results obtained

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:

来源