Dimethylamine → 4-acetyl-N,N-dimethylbenzene-1-sulfonamide

HRID 1194053

反応式

HRID 1194053 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10](Cl)(=[O:12])=[O:11])=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[CH3:14][NH:15][CH3:16]>C1COCC1>[CH3:14][N:15]([CH3:16])[S:10]([C:7]1[CH:8]=[CH:9][C:4]([C:1](=[O:3])[CH3:2])=[CH:5][CH:6]=1)(=[O:12])=[O:11]

参加物

4

反応物 2

HCID 674DimethylamineHCID 2664184-Acetylbenzenesulfonyl chloride

生成物 1

HCID 20640414-acetyl-N,N-dimethylbenzene-1-sulfonamide収率 93%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

p-Acetylbenzenesulphonyl chloride (4.0 g, 18 mmol), aqueous dimethylamine (10 ml, 55 mmol), and THF (30 ml) were stirred together for 1 h at 20° C. and then partitioned between ethyl acetate and brine. The organic layer was dried (MgSO4) and evaporated under reduced pressure and the resulting residue recrystallised from either water or ether to give p-dimethylaminosulphonylacetophenone as fine white needles (3.8 g, 93%) m.p. 98°-99° C. (H2O); δH (dmso-d6) 8.0 (4H, ABq, aryl), 2.65 (9H, S, 3×Me).

後処理

  1. custompartitioned between ethyl acetate and brine
  2. dry with materialThe organic layer was dried (MgSO4)
  3. customevaporated under reduced pressure
  4. customthe resulting residue recrystallised from either water or ether

出典と根拠

ORDレコード
ord-94090da0a78440cfbf0b943b1bebc324
出典データセット
uspto-grants-1989_03
特許番号
US04812470

関連ノート

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