HRID624206

反应详情

EQUATION

反应方程式

HRID 624206 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solution of methyl 6-aminopyridazine-3-carboxylate (14 g, 91.5 mmol) in anhydrous toluene (700 mL) was added Et3N (11.1, 109.8 mmol). A solution of triphosgene (27.2 g, 91.5 mmol) in anhydrous toluene was added slowly at 0° C. The reaction mixture was stirred for 2 hrs at room temperature and then heated at 90° C. for 5 hrs. After cooling to room temperature, toluene and water were added to the mixture, the mixture was separated and the organic layer was dried over anhydrous Na2SO4, concentrated under reduced pressure to give the title compound as a solid.

WORKUP

后处理

  1. temperatureheated at 90° C. for 5 hrs
  2. temperatureAfter cooling to room temperature
  3. customthe mixture was separated
  4. dry with materialthe organic layer was dried over anhydrous Na2SO4
  5. concentrationconcentrated under reduced pressure