反应 #1885066

反应方程式

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

12

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

oxalyl chloride

→

4-chloroquinazoline-6,7-diyl diacetate

溶剂

CHCl3

反应条件

后处理

1. 1
   其他The resulting reaction mixture
2. 2
   温度then was gradually heated
3. 3
   温度to reflux for 5 h during which time the starting material
4. 4
   其他was consumed
5. 5
   温度The reaction mixture was cooled to 10° C.
6. 6
   其他the solution was quenched with aq sodium bicarbonate
7. 7
   其他The organic layer was separated
8. 8
   洗涤washed with brine
9. 9
   干燥then dried over Na2SO4
10. 10
    浓缩directly taken to the next step without concentration

实验过程

To a solution of 6,7-diacetoxy-4(3H)-quinazolinone, 12 (3.20 g, 11.42 mmol) in CHCl3 (60 ml) was added oxalyl chloride (2.2 ml, 17.3 mmol) dropwise at 0° C. The resulting reaction mixture was stirred at room temperature for 15 minutes then was gradually heated to reflux for 5 h during which time the starting material was consumed. The reaction mixture was cooled to 10° C. and the solution was quenched with aq sodium bicarbonate. The organic layer was separated and washed with brine then dried over Na2SO4 and directly taken to the next step without concentration.

来源