Benzylamine → 4-Ethyl 3-methyl 1-benzyl-1,2-dihydro-2-oxopyridine-3,4-dicarboxylate

HRID 919711ノート

反応式

HRID 919711 の反応式
CO[C:3](=[O:20])[C:4]([C:16]([O:18][CH3:19])=[O:17])=[C:5]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH:6]=[CH:7][N:8]([CH3:10])C.C(N)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>CCO>[CH3:19][O:18][C:16]([C:4]1[C:3](=[O:20])[N:8]([CH2:10][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:7]=[CH:6][C:5]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[O:17]

参加物

4

反応物 2

HCID 7504BenzylamineHCID 851589875-Dimethylamino-3-ethoxycarbonyl-2-methoxycarbonyl-penta-2,4-dienoic acid methyl ester

生成物 1

HCID 682974044-Ethyl 3-methyl 1-benzyl-1,2-dihydro-2-oxopyridine-3,4-dicarboxylate収率 104.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 5-dimethylamino-3-ethoxycarbonyl-2-methoxycarbonyl-penta-2,4-dienoic acid methyl ester (5 g, 17.5 mmol) and benzylamine (2 mL, 18.4 mmol) in EtOH (30 mL) was refluxed for 5 h. The mixture was cooled to r.t., concentrated in vacuo, and taken up in ether. The solution was washed with 1M HCl and water, and then dried over MgSO4. Evaporation of the solvent in vacuo afforded 5.77 g of the title compound as a viscous orange oil. MS: (+) m/z 338.06 (M+Na).

後処理

  1. temperaturewas refluxed for 5 h
  2. concentrationconcentrated in vacuo
  3. washThe solution was washed with 1M HCl and water
  4. dry with materialdried over MgSO4
  5. customEvaporation of the solvent in vacuo

出典と根拠

ORDレコード
ord-e1b1b619a05842e891885dcc2d6971ef
出典データセット
uspto-grants-2016_03
特許番号
US09271970B2

反応ノート

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