Reaktion #4973

Reaktionsgleichung

3,5-di-(2,4-di-tert-amylphenoxypropylcarbamoyl)benzenesulfonyl chloride

sodium sulfite

sodium hydrogen carbonate

water

→

solid

Ausbeute 82.8%

sodium 3,5-di-(2,4-di-tert-amylphenoxypropylcarbamoyl)benzenesulfinate

Ausbeute 82.8%

Lösungsmittel

acetonitrile

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeobtained in the aforesaid step
2. 2
   workup.ADDITIONthe reaction mixture was poured onto ice water
3. 3
   Extraktionextracted with 150 ml of ethyl acetate
4. 4
   WaschenThe ethyl acetate layer was washed thrice with cold water
5. 5
   Trocknendried over Glauber's salt
6. 6
   FiltrationAfter filtrating away the Glauber's salt
7. 7
   Einengenthe residue was concentrated to dryness

Vorschrift

To 2 g (0.016 mol) of sodium sulfite and 2.4 g (0.029 mol) of sodium hydrogen carbonate were added 100 ml of water and 20 ml of acetonitrile and the mixture was stirred at 30° C. To the mixture was added dropwise a solution of 10.5 g (0.013 mol) of 3,5-di-(2,4-di-tert-amylphenoxypropylcarbamoyl)benzenesulfonyl chloride obtained in the aforesaid step dissolved in 100 ml of acetonitrile. After stirring the resultant mixture for one hour, the reaction mixture was poured onto ice water and extracted with 150 ml of ethyl acetate. The ethyl acetate layer was washed thrice with cold water and dried over Glauber's salt. After filtrating away the Glauber's salt, the residue was concentrated to dryness to provide 8.6 g (yield of 82.8%) of a solid product.

Quelle