反应 #4619

反应方程式

chloroacetone

potassium carbonate

chloroacetone

2,3-dihydro-2,2-dimethyl-6-hydroxy-4H-1,3-benzoxazin-4-one

→

2,3-dihydro-2,2-dimethyl-6-(2-oxopropoxy)-4H-1,3-benzoxazin-4-one

溶剂

acetonitrile

反应条件

后处理

1. 1
   温度the reaction mixture is heated for a further 15 to 20 hours
2. 2
   其他The still warm reaction mixture
3. 3
   过滤is filtered
4. 4
   洗涤the residue thoroughly washed with acetone
5. 5
   浓缩the combined filtrate is concentrated by evaporation
6. 6
   其他The crystalline residue is recrystallised from toluene

实验过程

70 g of 2,3-dihydro-2,2-dimethyl-6-hydroxy-4H-1,3-benzoxazin-4-one are refluxed for 30 hours, whilst stirring, in 400 ml of acetonitrile with 100 g of potassium carbonate and 32 ml of chloroacetone. After the addition of a further 3.2 ml of chloroacetone, the reaction mixture is heated for a further 15 to 20 hours. The still warm reaction mixture is filtered, the residue thoroughly washed with acetone and the combined filtrate is concentrated by evaporation. The crystalline residue is recrystallised from toluene and yields 2,3-dihydro-2,2-dimethyl-6-(2-oxopropoxy)-4H-1,3-benzoxazin-4-one having a melting point of 125°-126°.

来源