HRID1387279

反应详情

EQUATION

反应方程式

HRID 1387279 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-iodo-4-methyl-3-nitro-2-pyridone (2.90 g, 10.4 mmol) and sodium hydride (60% in oil, 0.44 g, 11 mmol) was stirred at rt for 2.5 hours. 4-Methoxybenzyl chloride (1.50 mL) was added, and the mixture was stirred at rt for 18 h. Water was added, and the l s mixture and extracted with ethyl acetate. The organic phase was washed, dried and evaporated. Chromatography of the residue over silica gel (35% ethyl acetate/petroleum ether) followed by crystallization from water gave 1-(4-methoxybenzyl)-5-iodo-4-methyl-3-nitro-2-pyridone (3.11 g, 75%).

WORKUP

后处理

  1. stirringthe mixture was stirred at rt for 18 h
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed
  4. customdried
  5. customevaporated
  6. customChromatography of the residue over silica gel (35% ethyl acetate/petroleum ether) followed by crystallization from water