HRID639033

反应详情

EQUATION

反应方程式

HRID 639033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 2-(hydroxymethyl)-5-({[4-(methoxy)phenyl]methyl}oxy)-4(1H)-pyrone (40 g, 153 mmol) in ethanol (105 mL) was added concentrated aqueous ammonia (295 mL) and refluxed for 18 hours. The mixture was cooled, then refrigerated for 3 hours, and cooled in an ice-bath for 45 minutes. The solid was filtered off, washed with cold ethanol, followed by cold petroleum ether and dried in vacuo to afford the product as brown solid (26.21 g, 66%).

WORKUP

后处理

  1. temperaturerefluxed for 18 hours
  2. temperatureThe mixture was cooled
  3. temperaturecooled in an ice-bath for 45 minutes
  4. filtrationThe solid was filtered off
  5. washwashed with cold ethanol
  6. customdried in vacuo