反应 #362533

反应方程式

methoxythioacetamide

2-chloroacetoacetic acid ethyl ester

water

→

2-methoxymethyl-4-methylthiazole-5-carboxylic acid ethyl ester

溶剂

benzene

ethyl acetate

反应条件

后处理

1. 1
   温度heated
2. 2
   温度under reflux for 41/2 hours
3. 3
   洗涤washed twice
4. 4
   干燥dried over sodium sulfate
5. 5
   过滤filtered
6. 6
   其他The solvent mixture is evaporated off
7. 7
   其他The yellow oil that remains is crystallised by trituration with diisopropyl ether
8. 8
   其他melt at 36°-37° C.

实验过程

20 g of methoxythioacetamide are added, with vigorous stirring, to 31.3 g of 2-chloroacetoacetic acid ethyl ester in 400 ml of benzene at room temperature and then, using a water separator, heated under reflux for 41/2 hours. After cooling to room temperature, the benzenic reaction solution is diluted with 500 ml of ethyl acetate, washed twice using 80 ml of 10% sodium carbonate solution each time and twice using 50 ml of water each time, dried over sodium sulfate and filtered. The solvent mixture is evaporated off. The yellow oil that remains is crystallised by trituration with diisopropyl ether. The beige-coloured crystals melt at 36°-37° C.

来源