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

HRID 1929302노트

반응식

HRID 1929302 반응식
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

참가 물질

4

반응물 2

HCID 962WaterHCID 12502457HCID 12502457, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-50907c63078445fbb22162bf191b09f2
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188069B2

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