HRID1428785

反应详情

EQUATION

反应方程式

HRID 1428785 的结构方程式

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

  1. temperatureThe mixture was refluxed for 6 h
  2. customAfter the starting material was consumed
  3. additiontreated with potassium bicarbonate to pH 12˜13
  4. extractionThen it was extracted with ethyl acetate
  5. washwashed with brine
  6. dry with materialDrying over magnesium sulfate, evaporation of the ethyl acetate and purification by column chromatography