Benzyl Chloride → 1-Benzyl-hexahydro-7-phenyl-1,4-diazepin-5-one

HRID 1637167노트

반응식

HRID 1637167 반응식
[C:1]1([CH:7]2[NH:13][CH2:12][CH2:11][NH:10][C:9](=[O:14])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:21](Cl)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C(#N)C>[CH2:21]([N:13]1[CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:8][C:9](=[O:14])[NH:10][CH2:11][CH2:12]1)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

참가 물질

5

반응물 3

HCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 130482357-Phenyl-1,4-diazepan-5-one

생성물 1

HCID 193479331-Benzyl-hexahydro-7-phenyl-1,4-diazepin-5-one수율 83.9%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

1.9 g hexahydro-7-phenyl-1,4-diazepin-5-one (for preparation see Example 1C) in 30 ml acetonitrile were heated to boiling with 2.0 g potassium carbonate and 1.2 g benzyl chloride with reflux cooling for 36 hours. Then filtration was carried out and the filtrate reduced in volume. The remaining residue was shaken with 10% aqueous citric acid solution, the organic phase was separated, dried over magnesium sulfate and reduced in volume under a vacuum. 2.23 g crude 1-benzyl-hexahydro-7-phenyl-1,4-diazepin-5-one were obtained as an oil, which was used for the next synthesis stage without further purification or characterization.

후처리

  1. temperaturewith reflux
  2. temperaturecooling for 36 hours
  3. filtrationThen filtration
  4. customthe organic phase was separated
  5. dry with materialdried over magnesium sulfate

출처 및 근거

ORD 기록
ord-6d0163b8cb4649f29ae48e11f811ce12
출처 데이터셋
uspto-grants-2000_03
특허 번호
US06040303

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