HRID1756052

反应详情

EQUATION

反应方程式

HRID 1756052 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 120 mg (0,37 mmol) of 3-chloro-2-metyl-7-phenacylpyrrolo[2,3-b]pyridine hydrochlorid in 2 ml methanol was added 30 mg (0,79mmol) of sodium borohydride. The mixture was stirred for 20 h at room temperature. The solvent was evaporated and the residue was partitioned between 2 ml of 0,2M hydrochloric acid and 2 ml of ethyl acetate. The aqueos layer was basified by addition of 2M sodium hydroxide and extracted twice with 2 ml of methylene chloride. The combined organic phase was dried over sodium sulfate and the solvent was evaporated. The residue was treated with acetonitrile and the precipitate was filtered off to give 20 mg (19%) 3-chloro-2-methyl-7-(2-phenyl-2-hydroxyethyl)pyrrolo-[2,3-b]pyridine.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. customthe residue was partitioned between 2 ml of 0,2M hydrochloric acid and 2 ml of ethyl acetate
  3. additionThe aqueos layer was basified by addition of 2M sodium hydroxide
  4. extractionextracted twice with 2 ml of methylene chloride
  5. dry with materialThe combined organic phase was dried over sodium sulfate
  6. customthe solvent was evaporated
  7. additionThe residue was treated with acetonitrile
  8. filtrationthe precipitate was filtered off