HRID734960

反应详情

EQUATION

反应方程式

HRID 734960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-[3-(1-methyl-1H-pyrazol-4-yl)-6-quinoxalinyl]-3-pyridinamine (52 g, 0.172 mmol) in pyridine (1.7 mL) was added 4-cyanobenzenesulfonyl chloride (56 mg, 0.278 mmol). The reaction mixture was stirred at room temperature overnight. Monitoring by LCMS still showed 30% of starting material. An additional portion of 4-cyanobenzenesulfonyl chloride (17 mg, 0.084 mmol) was added to the reaction mixture and after stirring for a further 30 minutes, all starting material was consumed. Cold water was poured into the reaction resulting in precipitate formation. This solid was collected by filtration, washed with water and dried under vacuum to give the title compound (54 mg, 67%) as a brown colored solid. MS(ES)+ m/e 468 [M+H]+.

WORKUP

后处理

  1. stirringafter stirring for a further 30 minutes
  2. customall starting material was consumed
  3. additionCold water was poured into the reaction
  4. customresulting in precipitate formation
  5. filtrationThis solid was collected by filtration
  6. washwashed with water
  7. customdried under vacuum