反应 #1806912

反应方程式

1-chloroethyl 5-(2,4-difluorophenyl)salicylate

sodium ethyl carbonate

→

1-(ethoxycarbonyloxy)ethyl 5-(2,4-difluorophenyl)salicylate

溶剂

DMF

反应条件

后处理

1. 1
   浓缩concentrated in vacuo
2. 2
   其他The concentrate is partitioned between ether/ethyl acetate
3. 3
   其他The organic layer is separated
4. 4
   萃取the aqueous layer is again extracted with ether
5. 5
   洗涤washed with water
6. 6
   其他by drying
7. 7
   浓缩concentration to the crude product
8. 8
   其他After further purification by chromatography
9. 9
   其他the product is crystallized from hexane

实验过程

To a solution of 1-chloroethyl 5-(2,4-difluorophenyl)salicylate (5.0 g) in about 40 ml of DMF is added portionwise 3.0 g of sodium ethyl carbonate. The reaction is stirred at room temperature and then concentrated in vacuo. The concentrate is partitioned between ether/ethyl acetate and acidified water. The organic layer is separated and the aqueous layer is again extracted with ether, the organic layers are pooled and washed with water followed by drying and concentration to the crude product. After further purification by chromatography as described in Example 1, the product is crystallized from hexane to afford pure 1-(ethoxycarbonyloxy)ethyl 5-(2,4-difluorophenyl)salicylate.

来源