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

HRID 1637167ノート

反応式

HRID 1637167 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-6d0163b8cb4649f29ae48e11f811ce12
出典データセット
uspto-grants-2000_03
特許番号
US06040303

反応ノート

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