反应 #1726666

反应方程式

N-[4-[(2-pyridinylamino)sulfonyl]phenyl]-acetamide

NaOH

→

4-amino-N-2-pyridinyl-benzenesulfonamide

收率 70.7%

溶剂

ethanol

1-methoxy-2-propanol

—

mixture

反应条件

后处理

1. 1
   温度the mixture was refluxed for an hour
2. 2
   其他the solvent was removed under reduced pressure
3. 3
   workup.DISSOLUTIONThe residue was dissolved in 1300 ml water
4. 4
   其他The precipitated impurities were removed by filtration
5. 5
   萃取the aqueous fraction was extracted three times with 450 ml methylene chloride
6. 6
   其他4-amino-N-2-pyridinyl-benzenesulfonamide precipitated from the medium
7. 7
   其他was isolated by filtration
8. 8
   其他dried

实验过程

The isolated N-[4-[(2-pyridinylamino)sulfonyl]phenyl]-acetamide was dissolved in 2.5 l of a mixture of ethanol and 1-methoxy-2-propanol (1/1). 105 g (2.66 mol) NaOH was added and the mixture was refluxed for an hour. The reaction mixture was allowed to cool down to room temperature and the solvent was removed under reduced pressure. The residue was dissolved in 1300 ml water and the mixture was acidified to pH 1 using HCl (conc.). The precipitated impurities were removed by filtration and the aqueous fraction was extracted three times with 450 ml methylene chloride. The aqueous fraction was neutralized to pH 7, using a 10 N NaOH solution. 4-amino-N-2-pyridinyl-benzenesulfonamide precipitated from the medium, was isolated by filtration and dried. 93.4 g (70.7%) of 4-amino-N-2-pyridinyl-benzenesulfonamide was isolated.

来源