Lawesson's reagent → HCID 23289285, 화합물

HRID 366457노트

반응식

HRID 366457 반응식
[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]

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 22448959HCID 22448959, 화합물

생성물 1

HCID 23289285HCID 23289285, 화합물수율 135.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-029f2d7774424f75a42acb9381af448e
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06130217

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