1-(2-Methyl-5-nitro-phenyl)-piperidin-4-one → 3-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-one

HRID 1853945

反応式

HRID 1853945 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[N:11]1[CH2:16][CH2:15][C:14](=[O:17])[CH2:13][CH2:12]1>COC(OC)N(C)C>[CH3:3][N:11]([CH:16]=[C:13]1[C:14](=[O:17])[CH2:15][CH2:16][N:11]([C:3]2[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=2[CH3:1])[CH2:12]1)[CH3:12]

参加物

3

反応物 1

HCID 666567781-(2-Methyl-5-nitro-phenyl)-piperidin-4-one

生成物 1

HCID 673288983-Dimethylaminomethylene-1-(2-methyl-5-nitrophenyl)piperidin-4-one

試薬・触媒・溶媒 1

HCID 78373Dimethylformamide dimethyl acetal溶媒

実験手順

A solution of 1-(2-Methyl-5-nitro-phenyl)-piperidin-4-one [100 mg, 0.426 mmol] in N,N-Dimethylformamide dimethyl acetal (DMA.DMF) [1 ml] was heated to reflux for 12 hrs. After cooling to room temperature, reaction mixture was concentrated under vacuum. The dark brown crude product obtained was further purified by silica gel chromatography using 30-60% ethyl acetate/hexane as eluent to obtain pure desired product i.e., 3-Dimethylaminomethylene-1-(2-methyl-5-nitro-phenyl)-piperidin-4-one [4] as orange solid [Yield: 76.2 mg, 62.02%]

後処理

  1. temperatureto reflux for 12 hrs
  2. customreaction mixture
  3. concentrationwas concentrated under vacuum
  4. customThe dark brown crude product obtained
  5. customwas further purified by silica gel chromatography

出典と根拠

ORDレコード
ord-b2b4d79805b2495988cffa207aa2cc19
出典データセット
uspto-grants-2015_02
特許番号
US08962637B2

関連ノート

読み込み中…