Acetone → (3,4-Dichlorophenyl)methanesulfonamide

HRID 731393

反応式

HRID 731393 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][S:10](Cl)(=[O:12])=[O:11])[CH:5]=[CH:6][C:7]=1[Cl:8].CC(C)=O.[OH-].[NH4+:19]>O>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][S:10]([NH2:19])(=[O:12])=[O:11])[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

5

反応条件

温度
2.5 °C

実験手順

A solution of (3,4-dichloro-phenyl)-methanesulfonyl chloride (500 g, 1.93 mol) and acetone (470 mL) was added over 2 h to cooled (0-5° C.), stirred concentrated ammonium hydroxide (28%, 900 mL, 227 g NH3, 13.3 mol). The reaction mixture was maintained below 12° C. during the addition. The reaction mixture was allowed to warm to room temperature and was stirred for 1 h. Water (900 mL) was added to the reaction mixture and it was stirred for 1 h. The white solid was collected by filtration, washed with cold water (2×500 mL), and vacuum dried to give 375 g (81%) of (3,4-dichloro-phenyl)-methanesulfonamide with 99% purity (as determined by HPLC).

後処理

  1. temperatureThe reaction mixture was maintained below 12° C. during the addition
  2. temperatureto warm to room temperature
  3. stirringwas stirred for 1 h
  4. filtrationThe white solid was collected by filtration
  5. washwashed with cold water (2×500 mL), and vacuum
  6. customdried

出典と根拠

ORDレコード
ord-f0507f5963ea426db87d7ffd1d49254e
出典データセット
uspto-grants-2009_09
特許番号
US07582772B2

関連ノート

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