Acetyl chloride → 1-(6-Methoxy-2,2,4-trimethylquinolin-1(2H)-yl)ethan-1-one

HRID 557578ノート

反応式

HRID 557578 の反応式
[C:1](Cl)(=[O:3])[CH3:2].[CH3:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12]([CH3:18])([CH3:17])[CH:11]=[C:10]2[CH3:19]>N1C=CC=CC=1>[C:1]([N:13]1[C:14]2[C:9](=[CH:8][C:7]([O:6][CH3:5])=[CH:16][CH:15]=2)[C:10]([CH3:19])=[CH:11][C:12]1([CH3:18])[CH3:17])(=[O:3])[CH3:2]

参加物

4

実験手順

Acetyl chloride (8 ml) was added dropwise to a cooled (0° C.) solution of 1,2-dihydro-6-methoxy-2,2,4-trimethylquinoline (1.7 g) and a catalytic amount of N,N-dimethylaminopyridine in pyridine (60 ml). After stirring for 18 h, the reaction mixture was concentrated in vacuo. The residue was dissolved in dichloromethane and washed with 1 M HCl, water, 5% aq. NaHCO3, water and brine. The organic layer was dried (MgSO4) and concentrated in vacuo. The residue was chromatographed on silicagel in dichloromethane as eluent.

後処理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. dissolutionThe residue was dissolved in dichloromethane
  3. washwashed with 1 M HCl, water, 5% aq. NaHCO3, water and brine
  4. dry with materialThe organic layer was dried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe residue was chromatographed on silicagel in dichloromethane as eluent

出典と根拠

ORDレコード
ord-96ce798c83d84b84ae4661e9d921f60b
出典データセット
uspto-grants-2011_11
特許番号
US08058441B2

反応ノート

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