反应 #2510187

反应方程式

Oxalyl chloride

chloroform

6,7-diacetoxy-4(3H)-quinazolinone

→

4-Chloro-6,7-diacetoxy-quinazoline

溶剂

dimethylformamide

反应条件

后处理

1. 1
   温度reflux condenser
2. 2
   workup.ADDITIONaddition funnel
3. 3
   其他obtained by the process
4. 4
   温度The reaction mass was slowly heated
5. 5
   温度to reflux temperature
6. 6
   温度maintained
7. 7
   温度at reflux temperature for 6 hours
8. 8
   其他Reaction
9. 9
   其他slowly quenched into saturated sodium bicarbonate solution at less than 10° C
10. 10
    其他Separated the organic layer
11. 11
    干燥dried over anhydrous sodium sulfate
12. 12
    其他The dried organic layer thus obtained
13. 13
    其他was directly used in the next step without any purification

实验过程

Into a 3.0 L four necked round bottomed flask, equipped with a mechanical stirrer, reflux condenser, pressure equalizing addition funnel and thermometer socket are charged chloroform (1000 ml), 6,7-diacetoxy-4(3H)-quinazolinone (50 g) obtained by the process described in step (ii) above and dimethylformamide (2 ml). Oxalyl chloride (50 g) was slowly added in about 20-30 minutes. The reaction mass was slowly heated to reflux temperature and maintained at reflux temperature for 6 hours. Reaction was found to be over by HPLC. Cooled the reaction mass to 25-30° C. and slowly quenched into saturated sodium bicarbonate solution at less than 10° C. Separated the organic layer and dried over anhydrous sodium sulfate. The dried organic layer thus obtained was directly used in the next step without any purification.

来源