Water → 5-Phenyl-1,3-dihydro-2H-azepin-2-one

HRID 1929302ノート

反応式

HRID 1929302 の反応式
C(N(CC)[C:4]1[CH2:10][CH:9]=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:7]=[CH:6][N:5]=1)C.[OH2:19]>COCCO>[C:11]1([C:8]2[CH:7]=[CH:6][NH:5][C:4](=[O:19])[CH2:10][CH:9]=2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

4

反応物 2

HCID 962WaterHCID 12502457HCID 12502457、化合物

生成物 1

HCID 573498745-Phenyl-1,3-dihydro-2H-azepin-2-one

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

実験手順

The crude diethyl-(5-phenyl-3H-azepin-2-yl)-amine (12.47 g) is added to water (10.0 mL) and 2-methoxy-ethanol (40.0 mL) and the resulting mixture heated to reflux and stirred 4½ days. The volatiles are removed in vacuo and the residue diluted with dichloromethane and washed with 0.1N HCl (2×200 mL) and saturated aqueous NaHCO3 (2×200 mL). The organic layer is dried over Na2SO4 and concentrated in vacuo to give the crude title compound as a dark brown solid (9.63 g). This material is carried into the next reaction without further purification.

後処理

  1. temperaturethe resulting mixture heated
  2. temperatureto reflux
  3. customThe volatiles are removed in vacuo
  4. additionthe residue diluted with dichloromethane
  5. washwashed with 0.1N HCl (2×200 mL) and saturated aqueous NaHCO3 (2×200 mL)
  6. dry with materialThe organic layer is dried over Na2SO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-50907c63078445fbb22162bf191b09f2
出典データセット
uspto-grants-2012_05
特許番号
US08188069B2

反応ノート

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