تفاعل #1806912

معادلة التفاعل

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

sodium ethyl carbonate

→

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

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   تركيزconcentrated in vacuo
2. 2
   أخرىThe concentrate is partitioned between ether/ethyl acetate
3. 3
   أخرىThe organic layer is separated
4. 4
   استخلاصthe aqueous layer is again extracted with ether
5. 5
   غسيلwashed with water
6. 6
   أخرىby drying
7. 7
   تركيزconcentration to the crude product
8. 8
   أخرىAfter further purification by chromatography
9. 9
   أخرىthe product is crystallized from hexane

الإجراء التجريبي

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.

المصدر