HRID487718

反应详情

EQUATION

反应方程式

HRID 487718 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
61 °C

PROCEDURE

实验过程

The protected 2,6-di(methoxyacetamido)purine (IV) (1.55 kg, 2.20 mol) was dissolved in methanol (3.6 L) with stirring and warmed to 46°-48° C. A solution of sodium methoxide (30 g, 95%, 0.55 mol, in 250 mL methanol) was added and the solution was warmed to 61° C. The reaction was completed in about 1 hour (tlc) at which time the product started to precipitate. The mixture was allowed to cool to 30° C. and then refrigerated overnight. The product was collected, washed with ice-cold methanol (800 mL) and air-dried to give the title compound (V) 823 g (68%), mp 60°-62° C.

WORKUP

后处理

  1. temperaturewarmed to 46°-48° C
  2. customto precipitate
  3. temperatureto cool to 30° C.
  4. customrefrigerated overnight
  5. customThe product was collected
  6. washwashed with ice-cold methanol (800 mL)
  7. customair-dried