HRID457691

反应详情

EQUATION

反应方程式

HRID 457691 的结构方程式

PROCEDURE

实验过程

A solution of 2,6-dichloro-9-ethylpurine (2.7 g, 12.4 mmol), a compound of formula (2), in liquid ammonia (20 mL) was sealed in a stainless steel tube and set aside at room temperature for 20 hours. The solvent was removed in vacuo and the residue was purified by flash chromatography on a silica gel column eluting with EtOAc-cyclohexane (65:35) to give 2-chloro-9-ethyl-9H-purin-6-ylamine, a compound of formula (3) (2.28 g, 93%) as a chromatographically pure solid: mp 258–262° C.; 1H NMR (Me2SO-d6) δ 1.39 (t, 3H, J=7.3 Hz, CH2CH3), 4.13 (q, 2H, J=7.3 Hz, CH2CH3), 7.74 (s, 2H, NH2), 8.18 (s, 1H, H-8). Anal. (C7H7ClN5) C, H, N.

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. customthe residue was purified by flash chromatography on a silica gel column
  3. washeluting with EtOAc-cyclohexane (65:35)