HRID2201311
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customThe reaction was quenched with 2M HCl(aq)
- additiondiluted with EtOAc
- stirringthe mixture stirred overnight
- extractionThe mixture was then extracted with EtOAc (3×)
- washthe combined organic phases washed with brine
- dry with materialdried over sodium sulphate
- customevaporated under vacuum
- customThe residue was triturated with diethyl ether/hexane