HRID564727

反应详情

EQUATION

反应方程式

HRID 564727 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-(1,1-Dimethoxyethyl)-7-methoxyfuro[2,3-c]pyridine-4-carboxylic acid (0.66 g), p-nitrophenol (0.32 g), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.49 g) and 4-dimethylaminopyridine (catalytic) in dry dichloromethane (40 ml) were stirred overnight at room temperature. The mixture was diluted with dichloromethane (50 ml), washed with water (100 ml), dried over magnesium sulfate, filtered and the solvent removed in vacuo. Purification by column chromatography on silica eluting with 33% hexane in ethyl acetate to 100% ethyl acetate gave 2-(1,1-dimethoxyethyl)-7-methoxyfuro[2,3-c]pyridine-4-carboxylic acid 4-nitrophenyl ester (0.51 g) and 2-acetyl-7-methoxyfuro[2,3-c]pyridine-4-carboxylic acid 4-nitrophenyl ester (0.20 g) as white solids.

WORKUP

后处理

  1. washwashed with water (100 ml)
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. customthe solvent removed in vacuo
  5. customPurification by column chromatography on silica eluting with 33% hexane in ethyl acetate to 100% ethyl acetate