HRID1069624
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureto maintain
- temperaturereflux for 4 hours
- additionpoured off the catalyst
- washthe catalyst washed twice with methylene chloride
- filtrationThe combined solvents were filtered
- concentrationconcentrated
- customthe residue chromatographed on silica gel
- washon eluting with 10% MeOH/EtOAc