HRID1097664

反应详情

EQUATION

反应方程式

HRID 1097664 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (10 g, 0.044 mol) in anhydrous DMF (100 ml) was treated with iodoethane (5.4 ml, 0.068 mol) and Na2CO3 (4.9 g, 0.046 mol). The reaction mixture was left to stir at rt under nitrogen for 2 days. Iodoethane (0.35 ml, 0.0044 mol) was added and the mixture was left to stir at rt for 1 day. The mixture was partitioned between EtOAc and 2M HCl. The organic layer was separated, washed sequentially with saturated sodium sulphite solution and brine, dried (MgSO4) and concentrated. The crude solid was washed with Et2O to give the title compound as a white solid (8.37 g, 75%).

WORKUP

后处理

  1. waitThe reaction mixture was left
  2. waitthe mixture was left
  3. stirringto stir at rt for 1 day
  4. customThe mixture was partitioned between EtOAc and 2M HCl
  5. customThe organic layer was separated
  6. washwashed sequentially with saturated sodium sulphite solution and brine
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated
  9. washThe crude solid was washed with Et2O