HRID1805859
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
- 116 °C
PROCEDURE
实验过程
A mixture of 2-amino-5-benzyl-3H-pyrrolo[3,2-d]pyrimidin-4(5H)-one (1.1 g, 7.4 mmol) and POCl3 (7 mL, 74 mmol) was heated at 116° C. for 3 h. Upon completion of the reaction, the reaction mixture was poured into ice and extracted three times with ethyl acetate. The combined organic layers were washed with brine, dried over Na2SO4, filtered, and concentrated in vacuo. Purification by column chromatography, eluting with CH2Cl2/Acetone (3:1), afforded the product as a white solid (490 mg, 40%).
WORKUP
后处理
- customUpon completion of the reaction
- additionthe reaction mixture was poured into ice
- extractionextracted three times with ethyl acetate
- washThe combined organic layers were washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customPurification by column chromatography
- washeluting with CH2Cl2/Acetone (3:1)