HRID1069013

反应详情

EQUATION

反应方程式

HRID 1069013 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5.17 mL (3.65 g; 50 mmoles) of diethylamine in 20 mL of tetrahydrofuran was stirred and cooled in an ice bath, and a solution of 1.16 g (2.5 mmoles) of 4-Bromo-but-2-enoic acid [4-(3-bromo-phenylamino)-quinazolin-6-yl]-amide in 10 mL of tetrahydrofuran and 5 mL of N,N-dimethylformamide was added dropwise. After stirring for 2 hours, 45 mL of ethyl acetate and 30 mL of saturated aqueous sodium bicarbonate were added, and the layers were separated. The organic layer was extracted with 25 mL of brine, dried over sodium sulfate, and taken to an oil in vacuo. This was chromatographed on silica gel with 1:9 methanol methylene chloride to give 677 mg (59%) of the desired product, which melted at 196-199° C. Mass spectrum (m/e) M+2H 228.5.

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. customthe layers were separated
  3. extractionThe organic layer was extracted with 25 mL of brine
  4. dry with materialdried over sodium sulfate
  5. customThis was chromatographed on silica gel with 1:9 methanol methylene chloride