تفاعل #1726666

معادلة التفاعل

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

NaOH

→

4-amino-N-2-pyridinyl-benzenesulfonamide

المردود 70.7%

المذيبات

ethanol

1-methoxy-2-propanol

—

mixture

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was refluxed for an hour
2. 2
   أخرىthe solvent was removed under reduced pressure
3. 3
   workup.DISSOLUTIONThe residue was dissolved in 1300 ml water
4. 4
   أخرىThe precipitated impurities were removed by filtration
5. 5
   استخلاصthe aqueous fraction was extracted three times with 450 ml methylene chloride
6. 6
   أخرى4-amino-N-2-pyridinyl-benzenesulfonamide precipitated from the medium
7. 7
   أخرىwas isolated by filtration
8. 8
   أخرىdried

الإجراء التجريبي

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.

المصدر