Reaktion #1806912

Reaktionsgleichung

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

sodium ethyl carbonate

→

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

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated in vacuo
2. 2
   SonstigeThe concentrate is partitioned between ether/ethyl acetate
3. 3
   SonstigeThe organic layer is separated
4. 4
   Extraktionthe aqueous layer is again extracted with ether
5. 5
   Waschenwashed with water
6. 6
   Sonstigeby drying
7. 7
   Einengenconcentration to the crude product
8. 8
   SonstigeAfter further purification by chromatography
9. 9
   Sonstigethe product is crystallized from hexane

Vorschrift

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.

Quelle