HRID1097698

反应详情

EQUATION

反应方程式

HRID 1097698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

To a mixture of ethyl 5-(3-butyl-8-chloro-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-1-yl)pentanoate (120 mg, 0.32 mmol) and of N-hydroxy-2-pyridinecarboximidamide (50 mg, 0.36 mmol) in EtOH (2 ml) was added a 21% (w/v) solution of sodium ethoxide in EtOH (0.225 ml, 0.62 mmol) and then heated in a sealed vial in a microwave oven at 140° C. for 10 min. The cooled mixture was evaporated to dryness and the residue partitioned between chloroform (5 ml) and saturated aqueous ammonium chloride (5 ml). The organic phase was evaporated to dryness and the crude product subjected to purification by MDAP. Product containing fractions were combined and evaporated to dryness. The product was triturated to a solid in a small amount of diethyl ether then dried to reveal the title compound as a white solid (44 mg, 31%).

WORKUP

后处理

  1. customThe cooled mixture was evaporated to dryness
  2. customthe residue partitioned between chloroform (5 ml) and saturated aqueous ammonium chloride (5 ml)
  3. customThe organic phase was evaporated to dryness
  4. customthe crude product subjected to purification by MDAP
  5. additionProduct containing fractions
  6. customevaporated to dryness
  7. customThe product was triturated to a solid in a small amount of diethyl ether
  8. customthen dried