HRID639034

反应详情

EQUATION

反应方程式

HRID 639034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-(hydroxymethyl)-5-({[4-(methoxy)phenyl]methyl}oxy)-4(1H)-pyridinone (26 g, 0.1 mol) in pyridine (150 mL) was cooled to 5° C. and treated with acetyl chloride (10.48 ml, 0.149 mol). The reaction mixture was stirred and allowed to warm to room temperature then heated at 60° C. for 18 hours. Pyridine was evaporated under vacuum and the residue was triturated with water (250 mL), cooled in an ice-bath for 30 minutes. The solid formed was filtered off, washed with cold water and dried in vacuo to afford the product as a solid (15.7 g, 50%); MS (+ve ion electrospray) m/z 304 (MH+).

WORKUP

后处理

  1. temperaturethen heated at 60° C. for 18 hours
  2. customPyridine was evaporated under vacuum
  3. customthe residue was triturated with water (250 mL)
  4. temperaturecooled in an ice-bath for 30 minutes
  5. customThe solid formed
  6. filtrationwas filtered off
  7. washwashed with cold water
  8. customdried in vacuo