HRID1441717

反应详情

EQUATION

反应方程式

HRID 1441717 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

468 mg (9.8 mMol) of 50% sodium hydride in oil were added at 0° C. to a solution of 1.0 g (3.9 mMol) of 3-(1-methyl-1,2,3,6-tetrahydropyridine-4-yl)-5-nitro-1H-indole in 50 ml of anhydrous dimethylformamide, and the mixture was left to stir for 30 minutes. Then 2.14 g of cyclohexanesulfonyl chloride were added, and the stirring continued for 3 hours at room temperature. Water was added and evaporated to dryness. The resulting crude was treated with sodium bicarbonate and was extracted with chloroform. The organic phase was dried with anhydrous sodium sulfate and evaporated to dryness; the resulting solid was purified by chromatography, obtaining 900 mg (57%) of 1-cyclohexanesulfonyl-3-(1-methyl-1,2,3,6-tetrahydropyridine-4-yl)-5-nitro-1H-indole as a yellow solid.

WORKUP

后处理

  1. waitthe mixture was left
  2. waitthe stirring continued for 3 hours at room temperature
  3. customevaporated to dryness
  4. additionThe resulting crude was treated with sodium bicarbonate
  5. extractionwas extracted with chloroform
  6. dry with materialThe organic phase was dried with anhydrous sodium sulfate
  7. customevaporated to dryness
  8. customthe resulting solid was purified by chromatography