HRID564729

反应详情

EQUATION

反应方程式

HRID 564729 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-amino-3,5-dichloropyridine (57 mg) in dry N,N-dimethylformamide (10 ml) was stirred at room temperature under an atmosphere of dry nitrogen. Sodium hydride (21 mg) was added and stirring continued for 45 minutes. 2-Acetyl-7-methoxyfuro[2,3-c]pyridine-4-carboxylic acid 4-nitrophenyl ester (100 mg) was added and the resulting mixture stirred overnight. The solvent was removed in vacuo, the residue taken up in water (100 ml) and extracted with ethyl acetate (3×100 ml). The combined organic extracts were washed with water (100 ml) then brine (50 ml), dried over magnesium sulfate, filtered and the solvent removed in vacuo. Purification by column chromatography on silica eluting with 50% hexane in ethyl acetate gave the title compound (12 mg) as a white solid.

WORKUP

后处理

  1. stirringthe resulting mixture stirred overnight
  2. customThe solvent was removed in vacuo
  3. extractionextracted with ethyl acetate (3×100 ml)
  4. washThe combined organic extracts were washed with water (100 ml)
  5. dry with materialbrine (50 ml), dried over magnesium sulfate
  6. filtrationfiltered
  7. customthe solvent removed in vacuo
  8. customPurification by column chromatography on silica eluting with 50% hexane in ethyl acetate