HRID850058

反应详情

EQUATION

反应方程式

HRID 850058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-(bromopentyloxy)benzamide (500 mg, 1.7 mmols), 6-chloropurine (270 mg, 1.7 mmols) and potassium carbonate (240 mg, 1.7 mmols) in DMF (7.5 ml) was stirred for two days at room temperature. The solvent was then removed under vacuum (0.001 mmHg) and the white solid (mixture of N7 and N9 isomers) was chromatographed (silica, 10% MeOH/CH2CI2) to give a single product (N9 isomer) as a glass. This was triturated with ether (~5 ml) to give a white solid which was recrystallised from ethyl acetate to give the product (120 mg, 0.33 mmols, 20% yield)

WORKUP

后处理

  1. customThe solvent was then removed under vacuum (0.001 mmHg)
  2. additionthe white solid (mixture of N7 and N9 isomers)
  3. customwas chromatographed (silica, 10% MeOH/CH2CI2)
  4. customto give a single product (N9 isomer) as a glass
  5. customThis was triturated with ether (~5 ml)
  6. customto give a white solid which
  7. customwas recrystallised from ethyl acetate