Phosphorus oxychloride → 2-Naphthalenesulfonyl chloride, 5-(acetylamino)-1-(acetyloxy)-
反応式
[C:1]([O:4][C:5]1[C:14]2[C:9](=[C:10]([NH:15][C:16]([CH3:18])=[O:17])[CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][C:6]=1[S:19]([OH:22])(=O)=[O:20])(=[O:3])[CH3:2].S1(CCCC1)(=O)=O.P(Cl)(Cl)([Cl:32])=O>>[C:1]([O:4][C:5]1[C:14]2[C:9](=[C:10]([NH:15][C:16]([CH3:18])=[O:17])[CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][C:6]=1[S:19]([Cl:32])(=[O:22])=[O:20])(=[O:3])[CH3:2]参加物
4
反応条件
- 温度
- 40 °C
実験手順
100 g of 1-acetoxy-5-acetaminonaphthalene-2-sulfonic acid was added to 500 ml of sulfolane, and 200 ml of phosphorus oxychloride was dropwise added thereto at 40° C. while stirring. After continuing stirring for about 1 hour, the reaction mixture was poured into 2 liters of ice water, and the precipitated crystals were collected by filtration, washed with water until the filtrate did not show acidity, and air-dried as such for 24 hours to obtain 70 g (81% yield) of product.