反应 #343498

反应方程式

6-ethyl-7-methoxy-5-methylimidazo[1,2-a]pyrimidine-2-carboxaldehyde

hydroxylamine-o-sulfonic acid

→

6-ethyl-7-methoxy-5-methylimidazo [1,2-a]pyrimidine-2-carbonitrile

收率 83.0%

溶剂

water

water

反应条件

后处理

1. 1
   其他After 40 minutes when the intermediate had precipitated
2. 2
   workup.ADDITION8 g of solid sodium hydroxide were added
3. 3
   workup.DISSOLUTIONthe intermediate dissolved
4. 4
   其他After 1 hour when the product had precipitated
5. 5
   过滤the mixture was filtered
6. 6
   洗涤the solid was washed with water
7. 7
   其他dried
8. 8
   其他crystallized from ethyl acetate

实验过程

To a rapidly stirred suspension of 19.84 g of 6-ethyl-7-methoxy-5-methylimidazo[1,2-a]pyrimidine-2-carboxaldehyde in 300 ml of water at room temperature was added all at once a solution of 13.30 g of hydroxylamine-o-sulfonic acid in 250 ml of water. After 40 minutes when the intermediate had precipitated, 8 g of solid sodium hydroxide were added and the intermediate dissolved. After 1 hour when the product had precipitated, the mixture was filtered and the solid was washed with water, dried, then crystallized from ethyl acetate to obtain 16.18 g of 6-ethyl-7-methoxy-5-methylimidazo [1,2-a]pyrimidine-2-carbonitrile (83% yield) as a pale yellow solid melting at 166°-168° C.

来源