HRID1640917

反应详情

EQUATION

反应方程式

HRID 1640917 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add Raney Nickel (1.38 g, 2.35 mmol) into a solution of 3-(1-azido-ethyl)-4-benzo[b]thiophen-7-yl-pyridine (0.66 g, 2.35 mmol) in ethanol (10 mL), formic acid (1.08 g, 23.54 mmol), and hydrazine (754.4 mg, 23.54 mmol) in a 50-mL round bottom flask in an ice bath. Stir the mixture at RT for 1 h and filter the Raney Nickel. Dilute the filtrate with ammonium hydroxide. Extract the product into chloroform. Wash the organic phase with water, dry over sodium sulfate, and concentrate to give the title compound as a brown oil (0.6 g, 100%). MS (ES) m/z 255 [M+1]+.

WORKUP

后处理

  1. filtrationfilter the Raney Nickel
  2. additionDilute the filtrate with ammonium hydroxide
  3. extractionExtract the product into chloroform
  4. washWash the organic phase with water
  5. dry with materialdry over sodium sulfate
  6. concentrationconcentrate