Salicylic Acid → 5-(Chlorosulfonyl)-2-hydroxybenzoic acid
反応式
[Cl:1][S:2]([OH:5])(=O)=[O:3].[C:6]([OH:15])(=[O:14])[C:7]1[C:8](=[CH:10][CH:11]=[CH:12][CH:13]=1)[OH:9]>>[Cl:1][S:2]([C:12]1[CH:11]=[CH:10][C:8]([OH:9])=[C:7]([CH:13]=1)[C:6]([OH:15])=[O:14])(=[O:5])=[O:3]参加物
3
実験手順
To 3.26 mol chlorosulfonic acid at 0° C. was added 652 mmol salicylic acid in small portions and the mixture was then allowed to stir at RT for 1 h, then at 50° C. for 1 h, and finally at 70° C. for 1 h. The mixture was then added dropwise to 1000 ml ice-water with stirring and stirring continued for an additional 30 min. The ensuing white crystals were collected by filtration, washed three times with water, and then dried in vacuo at 45° C. for 16 h to yield the title compound. MS (m/e): 236.8 ([{37Cl}M−H]−, 33%), 235.0 ([{37Cl}M−H]−, 100%)
後処理
- waitat 50° C. for 1 h
- waitfinally at 70° C. for 1 h
- stirringwith stirring
- stirringstirring
- waitcontinued for an additional 30 min
- filtrationThe ensuing white crystals were collected by filtration
- washwashed three times with water
- customdried in vacuo at 45° C. for 16 h
出典と根拠
- ORDレコード
- ord-d531d11ae1bd436fb38eba14b5f26270
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07557114B2
反応ノート
読み込み中…