HRID1428785
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a solution of 2-(2-fluoro-4-nitrobenzyl)isoindoline-1,3-dione (1.35 g, 4.48 mmol) in tetrahydrofurane 65% hydrazine monohydrate (1.3 mL, 4 eq) was added. The mixture was refluxed for 6 h. After the starting material was consumed, the mixture was cooled down to room temperature and treated with potassium bicarbonate to pH 12˜13. Then it was extracted with ethyl acetate and washed with brine. Drying over magnesium sulfate, evaporation of the ethyl acetate and purification by column chromatography gave (2-fluoro-4-nitrophenyl)methanamine (316 mg, 41%).
WORKUP
后处理
- temperatureThe mixture was refluxed for 6 h
- customAfter the starting material was consumed
- additiontreated with potassium bicarbonate to pH 12˜13
- extractionThen it was extracted with ethyl acetate
- washwashed with brine
- dry with materialDrying over magnesium sulfate, evaporation of the ethyl acetate and purification by column chromatography