Hydrochloric Acid → 4-Chloro-3-(chlorosulphonyl)benzoic acid
反応式
[Cl:1][S:2]([OH:5])(=O)=[O:3].[Cl:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=1.Cl>O>[Cl:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][C:8]=1[S:2]([Cl:1])(=[O:5])=[O:3]参加物
5
実験手順
28.05 kg (16 l) of chlorosulfonic acid are initially introduced and 4.4 kg of 4-chlorobenzoic acid were added in the course of 10 minutes with stirring (no heat effect). In the course of 90 minutes, the mixture was heated to 130-135° C., during which evolution of HCl was to be observed. The mixture was subsequently stirred for 3 hours at the stated temperature, and allowed to cool and to stand overnight. The reaction mixture was then allowed to run with stirring onto a mixture of 70 kg of ice and 30 kg of water, during which the temperature must not climb above 10° C. The product was filtered off with suction, washed with 40 kg of water and dried in vacuo at 40° C.
後処理
- stirringThe mixture was subsequently stirred for 3 hours at the stated temperature
- temperatureto cool
- customclimb above 10° C
- filtrationThe product was filtered off with suction
- washwashed with 40 kg of water
- customdried in vacuo at 40° C.
出典と根拠
- ORDレコード
- ord-cf9417b569df4750a0f842de6adaa6f3
- 出典データセット
- uspto-grants-2000_02
- 特許番号
- US06022899
反応ノート
読み込み中…