反応 #4973

反応方程式

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

sodium sulfite

sodium hydrogen carbonate

water

→

solid

収率 82.8%

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

収率 82.8%

溶媒

acetonitrile

acetonitrile

反応条件

後処理

1. 1
   その他obtained in the aforesaid step
2. 2
   workup.ADDITIONthe reaction mixture was poured onto ice water
3. 3
   抽出extracted with 150 ml of ethyl acetate
4. 4
   洗浄The ethyl acetate layer was washed thrice with cold water
5. 5
   乾燥dried over Glauber's salt
6. 6
   ろ過After filtrating away the Glauber's salt
7. 7
   濃縮the residue was concentrated to dryness

実験手順

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.

出典