HRID60356

反应详情

EQUATION

反应方程式

HRID 60356 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

To a solution of 3-(1-methyl-2,4-dioxo-1H-pyrrolo[3,2-d]pyrimidin-3(2H,4H,5H)-yl)propyl acetate (52 mg, 0.2 mmol) in DMF (3 mL) was added 1-chloro-4-(chloromethyl)benzene (64 mg, 0.4 mmol) and K2CO3 (82 mg, 0.6 mmol). The reaction was heated at 85° C. for 2 h, cooled to RT then diluted with EA (30 mL) and water (20 mL). The organic layer was washed with aq. 1N LiCl solution (3×10 mL), dried over Na2SO4 and concentrated to give 3-(5-(4-chlorobenzyl)-1-methyl-2,4-dioxo-1H-pyrrolo[3,2-d]pyrimidin-3(2H,4H,5H)-yl)propyl acetate (47 mg, 59% yield) as a solid. LCMS: MH+ 390 and TR=1.399 min. Used without further purification.

WORKUP

后处理

  1. temperaturecooled to RT
  2. washThe organic layer was washed with aq. 1N LiCl solution (3×10 mL)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated