HRID1719730
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
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.
WORKUP
后处理
- concentrationconcentrated in vacuo
- customThe concentrate is partitioned between ether/ethyl acetate
- customThe organic layer is separated
- extractionthe aqueous layer is again extracted with ether
- washwashed with water
- customby drying
- concentrationconcentration to the crude product
- customAfter further purification by chromatography
- customthe product is crystallized from hexane