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Methanesulfonyl chloride → HCID 10472404、化合物

HRID 1087205
ノート
印刷プレビュー

反応式

HRID 1087205 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[NH: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]>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]([NH: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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 10378008HCID 10378008、化合物

生成物 1

HCID 10472404HCID 10472404、化合物収率 58.9%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 4'-amino-3'-(2,4-difluorophenylamino)acetophenone (1.7 g) and methanesulfonyl chloride (0.9 g) in pyridine (17 ml) was stirred for 4 hours at room temperature. Pyridine was evaporated and the residue was stirred with an aqueous solution of sodium hydroxide (5%) for 30 minutes. The solution was washed with toluene, acidified to pH 3 with hydrochloric acid, and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium bicarbonate, dried, and concentrated under reduced pressure. The syrupy residue (1.8 g) was crystallized from ethanol to give pale yellow crystals of 4'-acetyl-2'-(2,4-difluorophenylamino)methanesulfonanilide (1.3 g).

後処理

  1. customPyridine was evaporated
  2. stirringthe residue was stirred with an aqueous solution of sodium hydroxide (5%) for 30 minutes
  3. washThe solution was washed with toluene
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with an aqueous solution of sodium bicarbonate
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. customThe syrupy residue (1.8 g) was crystallized from ethanol

出典と根拠

ORDレコード
ord-d9434fbdde084013836e46ee42d0a47a
出典データセット
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05034417

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート