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

HRID 1194053

반응식

HRID 1194053 반응식
[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]

참가 물질

4

반응물 2

HCID 674DimethylamineHCID 2664184-Acetylbenzenesulfonyl chloride

생성물 1

HCID 20640414-acetyl-N,N-dimethylbenzene-1-sulfonamide수율 93%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-94090da0a78440cfbf0b943b1bebc324
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04812470

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