反応式
[OH-].[Na+].[NH2:3][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]([S:14]([OH:17])(=[O:16])=[O:15])=[CH:6][CH:5]=1.[N:18]([O-])=O.[Na+].[ClH:22]>O>[ClH:22].[NH:3]([C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]([S:14]([OH:17])(=[O:15])=[O:16])=[CH:6][CH:5]=1)[NH2:18]参加物
6
反応条件
- 温度
- 0 °C
実験手順
4 g of NaOH are added to a suspension of 22.33 g of 4-amino-1-naphthalenesulphonic acid in 125 ml of water. The mixture is cooled to 0° C. and 2 ml of concentrated NaOH are added, followed by 7.5 g of sodium nitrite and 125 g of ice to maintain the temperature at 0° C. The suspension thereby obtained is poured into 75 ml of concentrated HCl cooled beforehand to 0° C., and left stirring for 2 hours 15 minutes at this temperature. The reaction mixture is added slowly to a solution, cooled beforehand to -10° C., of 55 g of stannous chloride dihydrate in 50 ml of concentrated HCl and 25 ml of water. After one night, the expected product is obtained by filtration, rinsing with 1N HCl and with water, m=23.96 g.
後処理
- temperatureto maintain the temperature at 0° C
- customThe suspension thereby obtained
- temperaturecooled beforehand to 0° C.
- waitleft
- additionThe reaction mixture is added slowly to a solution
- waitAfter one night
出典と根拠
- ORDレコード
- ord-44b64973a4d6423791beb8aa4ff8b6c6
- 出典データセット
- uspto-grants-1996_06
- 特許番号
- US05523455
関連ノート
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