Lawesson's reagent → HCID 23289285、化合物

HRID 366457ノート

反応式

HRID 366457 の反応式
[C:1]([O:4][C:5]1[C:10]2[CH2:11][CH2:12][CH2:13][C:14](=O)[NH:15][C:9]=2[CH:8]=[CH:7][CH:6]=1)(=[O:3])[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:26])=CC=1>C1(C)C=CC=CC=1>[C:1]([O:4][C:5]1[C:10]2[CH2:11][CH2:12][CH2:13][C:14](=[S:26])[NH:15][C:9]=2[CH:8]=[CH:7][CH:6]=1)(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 22448959HCID 22448959、化合物

生成物 1

HCID 23289285HCID 23289285、化合物収率 135.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A suspension of 1,3,4,5-tetrahydro-6-acetoxy-2H-1-benzazepin-2-one (50 mg, 0.23 mmol) and Lawesson reagent (65 mg, 0.16 mmol) in 3 mL of toluene was refluxed for about 1 h. The residue obtained after evaporation of the solvent was chromatographed on silica gel PTLC (5% MeOH--CH2Cl2) to give 51 mg (94%) of 1,3,4,5-tetrahydro-6-acetoxy-2H-1-benzazepin-2-thione; MS 235.

後処理

  1. temperaturewas refluxed for about 1 h
  2. customThe residue obtained
  3. customafter evaporation of the solvent
  4. customwas chromatographed on silica gel PTLC (5% MeOH--CH2Cl2)

出典と根拠

ORDレコード
ord-029f2d7774424f75a42acb9381af448e
出典データセット
uspto-grants-2000_10
特許番号
US06130217

反応ノート

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