HRID981192

反应详情

EQUATION

反应方程式

HRID 981192 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 6.17 g of ethyl 3-(2-chloro-6,7-difluoro-3-quinolyl)-3-oxopropionate in 7.15 g of N,N-dimethylformamide dimethyl acetal and 60 cm3 of ethyl acetate is heated at a temperature close to 75° C. for 1 hour 15 minutes. The reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at about 50° C. The residue is taken up in 50 cm3 of diisopropyl ether, drained and washed with 3 times 25 cm3 of the same solvent. 6.65 g of ethyl 2-(2-chloro-6,7-difluoroquinoline-3-carbonyl)-3-dimethylaminoacrylate are obtained in the form of an orange solid melting at 140° C.

WORKUP

后处理

  1. temperatureis heated at a temperature
  2. customclose to 75° C. for 1 hour 15 minutes
  3. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at about 50° C
  4. washwashed with 3 times 25 cm3 of the same solvent