HRID1069624

反应详情

EQUATION

反应方程式

HRID 1069624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 230mg (0.63 mmol) of 4-(2-hydrazino-2-oxoethoxy)-2-methyl-1-(phenylmethyl)-1H-indole-3-acetamide and 300 mg of Raney Ni in 40 mL of ethanol was heated to maintain reflux for 4 hours. The mixture was cooled the EtOH poured off the catalyst, and the catalyst washed twice with methylene chloride. The combined solvents were filtered, concentrated and the residue chromatographed on silica gel and on eluting with 10% MeOH/EtOAc, 25 mg (11% yield) of 4-(2-amino-2-oxoethoxy)-2-methyl-1-(phenylmethyl)-1H-indole-3-acetamide were obtained. This material melted at 190-207° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto maintain
  3. temperaturereflux for 4 hours
  4. additionpoured off the catalyst
  5. washthe catalyst washed twice with methylene chloride
  6. filtrationThe combined solvents were filtered
  7. concentrationconcentrated
  8. customthe residue chromatographed on silica gel
  9. washon eluting with 10% MeOH/EtOAc