Hydrochloric Acid → Methanesulfonamide, N-[4-acetyl-2-[(2,4-difluorophenyl)thio]phenyl]-

HRID 1087204ノート

反応式

HRID 1087204 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][C:3]=1[S:11][C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=1[F:19].[CH3:20][S:21](Cl)(=[O:23])=[O:22].Cl>N1C=CC=CC=1>[C:8]([C:5]1[CH:6]=[CH:7][C:2]([NH:1][S:21]([CH3:20])(=[O:23])=[O:22])=[C:3]([S:11][C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=2[F:19])[CH:4]=1)(=[O:10])[CH3:9]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 31297Methanesulfonyl chlorideHCID 10062143HCID 10062143、化合物

生成物 1

HCID 10450972Methanesulfonamide, N-[4-acetyl-2-[(2,4-difluorophenyl)thio]phenyl]-収率 50.8%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 4'-amino-3'-(2,4-difluorophenylthio)acetophenone (2.0 g) and methanesulfonyl chloride (1.0 g) in pyridine (20 ml) was stirred overnight at room temperature. The mixture was poured into cold diluted hydrochloric acid and extracted with ethyl acetate. The extract was washed with water, dried, and concentrated under reduced pressure. The residue was recrystallized from ethanol to give yellow crystals of 4'-acetyl-2'-(2,4-difluorophenylthio)methanesulfonanilide (1.3 g).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-c57670d4ca4945e49f31d86191f8eb9c
出典データセット
uspto-grants-1991_07
特許番号
US05034417

反応ノート

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