HRID1295468

反应详情

EQUATION

反应方程式

HRID 1295468 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6-chloro-8-(2,5-dimethoxybenzyl)-N9-butyl purine (1 mmol) in dioxane was added 28% NH4OH (50 mmol) and the mixture was then heated at 100 C in a seal tube for 48 h. Solvent was removed by azeotrope distillation with toluene. Purification on a silica gel column (see above) gave pure 8-(2,5-dimethoxybenzyl)-9-butyl adenine, 1.1. Rf=0.35 in 5% MeOH in EtOHAc. 1H NMR (DMSO-d6) δ 8.08 (s, 1H), 7.04 (br s, 2H), 6.94 (d, 1H), 6.80 (dd, 1H), 6.66 (d, 1H), 4.14 (s, 2H), 4.04 (t, 2H), 3.72 (s, 3H), 3.63 (s, 3H), 1.52 (m, 2H), 1.22 (m, 2H), 0.82 (t, 3H).

WORKUP

后处理

  1. temperaturethe mixture was then heated at 100 C in a seal tube for 48 h
  2. customSolvent was removed by azeotrope distillation with toluene
  3. customPurification on a silica gel column (see above)