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4-Fluorophenylhydrazine hydrochloride → HCID 67206078, 화합물

HRID 2366564
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HRID 2366564 반응식
O=[C:2]1[CH2:7][CH2:6][CH:5]([NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:4][CH2:3]1.Cl.[F:20][C:21]1[CH:26]=[CH:25][C:24]([NH:27]N)=[CH:23][CH:22]=1>CC(O)=O.CC(=O)OCC>[F:20][C:21]1[CH:22]=[C:23]2[C:24](=[CH:25][CH:26]=1)[NH:27][C:2]1[CH2:7][CH2:6][CH:5]([NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:4][C:3]2=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 699814-Fluorophenylhydrazine hydrochlorideHCID 14615292Benzyl (4-oxocyclohexyl)carbamate

생성물 1

HCID 67206078HCID 67206078, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of benzyl (4-oxocyclohexyl)carbamate (21.7 g, 87.8 mmol) and 4-fluorophenylhydrazine hydrochloride (14.3 g, 87.8 mmol) in glacial AcOH (148 ml) was stirred at reflux for 1 h30. After cooling to rt, the reaction mixture was diluted with EA and washed with sat.aq. NaHCO3 solution. The aqueous phase was extracted twice with EA, the combined organic extracts were washed with sat. aq. NaHCO3 solution, water and brine, dried over MgSO4, filtered and concentrated in vacuo to give the title compound as a light brown foam which was used for the next step without further purification.

후처리

  1. temperatureat reflux for 1 h30
  2. washwashed with sat.aq
  3. extractionThe aqueous phase was extracted twice with EA
  4. washthe combined organic extracts were washed with sat. aq. NaHCO3 solution, water and brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-fa82c7a8886f4e02b6a2f53043e82dfd
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08697869B2

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