HRID344872

反应详情

EQUATION

反应方程式

HRID 344872 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

A suspension of ethyl 3-(2-chloro-6,7-difluoro-3-quinolyl)-3-oxopropionate (6.17 g) in N,N-dimethylformamide dimethyl acetal (7.15 g) and ethyl acetate (60 cc) is heated to a temperature in the region of 75° C. for 1 hour 15 minutes. The reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. The residue is taken up with isopropyl ether (50 cc), drained and washed with the same solvent (3×25 cc). Ethyl 2-(2-chloro-6,7-difluoro-3-quinolinecarbonyl)-3-(dimethyl amino)acrylate (6.65 g) is obtained in the form of an orange-colored solid, m.p. 140° C.

WORKUP

后处理

  1. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C
  2. washwashed with the same solvent (3×25 cc)