HRID1672122

反应详情

EQUATION

反应方程式

HRID 1672122 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

At 50° C. 12.5 g potassium carbonate and 16 g 8-methanesulphonyloxy-1,4-dioxa-spiro[4,5]decane (cf for example Journal of Medicinal Chemistry (1992), 35(12), 2243-7) are added to 18.1 g 4-[(3-chloro-2-fluoro-phenyl)amino]-6-hydroxy-7-methoxy-quinazoline (cf for example Bioorganic & Medicinal Chemistry Letters (2006), 16(18), 4908-4912) in 125 ml dimethylformamide and the mixture is stirred for 18 hours at 80° C. Another 4.7 g potassium carbonate and 4.0 g of 8-methanesulphonyloxy-1,4-dioxa-spiro[4,5]decane are added and the mixture is stirred for another 7 hours at 80° C. The reaction mixture is cooled, diluted with water and ethyl acetate and the precipitate formed is suction filtered and dried.

WORKUP

后处理

  1. customAt 50° C
  2. stirringthe mixture is stirred for another 7 hours at 80° C
  3. temperatureThe reaction mixture is cooled
  4. customthe precipitate formed
  5. filtrationfiltered
  6. customdried