HRID347846

反应详情

EQUATION

反应方程式

HRID 347846 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 tert-butyl N-[7-iodo-2-methylthiopyrazolo[1,5-a]pyridin-3-yl]carbamate (600 mg) in N,N-dimethylformamide (6 mL) was added sodium hydride (60% in oil; 80 mg) with ice bath, and the reaction mixture was stirred for 30 minutes at room temperature. (Bromomethyl)cyclopropane (0.22 mL) was added to the reaction mixture at the same temperature, and stirring was continued for 1 hour at 40° C. After completion of the reaction, the reaction mixture was gradually added to ice, extraction was performed with ethyl acetate, and the organic extract was washed with water and brine. The organic extract was dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure to afford a crude product of tert-butyl N-cyclopropylmethyl-N-[7-iodo-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-3-yl]carbamate.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 1 hour at 40° C
  3. customAfter completion of the reaction
  4. additionthe reaction mixture was gradually added to ice, extraction
  5. extractionthe organic extract
  6. washwas washed with water and brine
  7. extractionThe organic extract
  8. dry with materialwas dried over anhydrous magnesium sulfate
  9. customthe solvent was evaporated under reduced pressure