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2-Acetyl-1-tetralone → HCID 58948768, 화합물

HRID 1013016
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HRID 1013016 반응식
[C:1]([CH:4]1[CH2:13][CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]1=O)(=O)[CH3:2].Cl.[CH3:16][O:17][C:18]1[CH:23]=[CH:22][C:21]([NH:24][NH2:25])=[CH:20][CH:19]=1>C(O)C.O>[CH3:16][O:17][C:18]1[CH:23]=[CH:22][C:21]([N:24]2[C:5]3[C:6]4[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=4[CH2:12][CH2:13][C:4]=3[C:1]([CH3:2])=[N:25]2)=[CH:20][CH:19]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 865272-Acetyl-1-tetraloneHCID 27239044-Methoxyphenylhydrazine hydrochloride

생성물 1

HCID 58948768HCID 58948768, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

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온도
80 °C

실험 절차

To a solution of 2-acetyl-1-tetralone (329 mg, 1.75 mmol) in ethanol (12 mL) was added 4-methoxyphenyl hydrazine hydrochloride. The stirred suspension was heated to 80° C. overnight. The reaction was cooled to room temperature and diluted with water (100 mL) and extracted with EtOAc (2×50 mL). The combined organic layers were washed with water, 10% NaOH, 10% HCl, brine and dried over Na2SO4. The solvent was removed under reduced pressure and the residue purified on silica gel using a 5% EtOAc to 25% EtOAc in hexane gradient (yield 396 mg). LC-MS (C19H18N2O calculated 290) m/z 291 (M+H).

후처리

  1. temperatureThe reaction was cooled to room temperature
  2. extractionextracted with EtOAc (2×50 mL)
  3. washThe combined organic layers were washed with water, 10% NaOH, 10% HCl, brine
  4. dry with materialdried over Na2SO4
  5. customThe solvent was removed under reduced pressure
  6. customthe residue purified on silica gel using a 5% EtOAc to 25% EtOAc in hexane gradient (yield 396 mg)

출처 및 근거

ORD 기록
ord-c9c0a684e2754c58bd635fedd8cbcbb8
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981896B2

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