Ammonium Hydroxide → 2,3-Dichlorobenzenesulfonamide
反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[S:9](Cl)(=[O:11])=[O:10].[OH-].[NH4+:14]>O1CCCC1>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[S:9]([NH2:14])(=[O:11])=[O:10]参加物
4
実験手順
To a stirred solution of 60.0 g of 2,3-dichlorobenzenesulfonyl chloride in 500 mL of tetrahydrofuran at 0° C. was added 30 mL of concentrated ammonium hydroxide (30%) dropwise at a rate that maintained the temperature below 15° C. After an additional stirring period of 0.5 hr, the tetrahydrofuran was evaporated under reduced pressure. The resultant solid residue was triturated with 500 mL of water, filtered, and the collected solid washed twice with 100-mL portions of water and dried to yield 52 g of 2,3-dichlorobenzenesulfonamide as a tan solid, m.p. 210°-226° C.; IR (nujol): 3360, 3250, 1370, 1175, 1165 cm-1.
後処理
- temperaturemaintained the temperature below 15° C
- customthe tetrahydrofuran was evaporated under reduced pressure
- customThe resultant solid residue was triturated with 500 mL of water
- filtrationfiltered
- washthe collected solid washed twice with 100-mL portions of water
- customdried
出典と根拠
- ORDレコード
- ord-e038212b29fc4d82b0b4d1d85de1e186
- 出典データセット
- uspto-grants-1987_02
- 特許番号
- US04645527
反応ノート
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