HRID1517969

反应详情

EQUATION

反应方程式

HRID 1517969 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.4 g of 3-chloro-5-nitro-toluene are dissolved in 35 ml of ethanol, combined with 15.8 g tin dichloride-dihydrate and refluxed for 3 hours. The solvent is eliminated in vacuo, the residue is taken up in 4 M sodium hydroxide solution and filtered through kieselguhr. The filter cake is washed thoroughly with ethyl acetate. The aqueous phase is extracted 3 times with ethyl acetate and the combined organic phases are washed with saturated sodium chloride solution and dried on magnesium sulphate. The solvent is eliminated in vacuo and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 81:15 to 70:30).

WORKUP

后处理

  1. temperaturerefluxed for 3 hours
  2. filtrationfiltered through kieselguhr
  3. washThe filter cake is washed thoroughly with ethyl acetate
  4. extractionThe aqueous phase is extracted 3 times with ethyl acetate
  5. washthe combined organic phases are washed with saturated sodium chloride solution
  6. customdried on magnesium sulphate
  7. customthe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 81:15 to 70:30)