HRID1499377
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
To a mixture of 4 (0.326 g, 0.881 mmol), 3-nitrophthalic anhydride (0.211 g, 1.093 mmol) and sodium acetate (0.097 g, 1.181 mmol) was added acetic acid (4.0 mL) and the resulting mixture was stirred overnight at 130° C. After 20 h, the mixture was carefully neutralized with sodium bicarbonate and extracted into DCM. The organic layer was dried over MgSO4, filtered, and concentrated. Purification by flash chromatography (95:5 DCM:MeOH) afforded 5 (0.241 g, 54%) as a white solid.
WORKUP
后处理
- waitAfter 20 h
- extractionextracted into DCM
- dry with materialThe organic layer was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customPurification by flash chromatography (95:5 DCM:MeOH)