HRID618221

反应详情

EQUATION

反应方程式

HRID 618221 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 2,6-dinitro-m-xylene (11.2 g) and 10% palladium on charcoal (620 mg) was stirred in triethylamine (36 mL) under an atmosphere of nitrogen and heated to reflux. Formic acid (9.25 mL) was added dropwise to the above mixture with vigorous stirring. After addition, the mixture was allowed to stir at reflux for an additional 15 min, then cooled to room temperature. The reaction mixture was diluted with ethyl acetate (100 mL) and filtered through celite. The filtrate was washed with brine and dried over magnesium sulfate. Evaporation afforded 9.51 g as a yellow solid.

WORKUP

后处理

  1. temperatureheated to reflux
  2. additionAfter addition
  3. temperatureat reflux for an additional 15 min
  4. filtrationfiltered through celite
  5. washThe filtrate was washed with brine
  6. dry with materialdried over magnesium sulfate
  7. customEvaporation
  8. customafforded 9.51 g as a yellow solid