HRID2119206

反应详情

EQUATION

反应方程式

HRID 2119206 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

1.29 g (0.005 mole) 3,4-dihydro-2-methyl-4-oxo-2H-1,2-benzothiazine-3-carboxylic acid 1,1-dioxide and 4.18 ml triethylamine were dissolved in 15 ml tetrahydrofuran and the mixture cooled to -5° C. and 1.91 ml benzenesulfonyl chloride was added slowly to the stirred mixture and stirred, and after one hour 0.52 g 2-aminopyridine was added to the mixture. The temperature of the mixture was raised slowly to ambient temperature and stirred for 4 hours, and twice the volume of ice water was added to the mixture to form precipitates. The obtained precipitates were filtered and recrystallized in ethanol and ethylether to obtain 1.6 g of the title compound. Yield: 68%. m.p 192°-195° C.

WORKUP

后处理

  1. temperatureThe temperature of the mixture was raised slowly to ambient temperature
  2. stirringstirred for 4 hours
  3. customto form
  4. customprecipitates
  5. customThe obtained precipitates
  6. filtrationwere filtered
  7. customrecrystallized in ethanol