HRID2201311

反应详情

EQUATION

反应方程式

HRID 2201311 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Phosphorous oxychloride (1.081 mL, 11.60 mmol) was added slowly to a solution of 1,3-dimethyl-5-phenyl-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione (2.96 g, 11.60 mmol) in DMF (40 mL) at 0° C. The mixture was stirred at 0° C. for 15 mins. The reaction was quenched with 2M HCl(aq), diluted with EtOAc, and the mixture stirred overnight. The mixture was then extracted with EtOAc (3×) and the combined organic phases washed with brine, dried over sodium sulphate and evaporated under vacuum. The residue was triturated with diethyl ether/hexane to afford the title compound.

WORKUP

后处理

  1. customThe reaction was quenched with 2M HCl(aq)
  2. additiondiluted with EtOAc
  3. stirringthe mixture stirred overnight
  4. extractionThe mixture was then extracted with EtOAc (3×)
  5. washthe combined organic phases washed with brine
  6. dry with materialdried over sodium sulphate
  7. customevaporated under vacuum
  8. customThe residue was triturated with diethyl ether/hexane