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Ammonium Acetate → 1-Amino-5-(5-chloro-2-fluorophenyl)cyclohexan-3-one

HRID 1700702
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인쇄 미리보기

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HRID 1700702 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([F:16])=[C:6]([CH:8]2[CH2:13][C:12](=O)[CH2:11][C:10](=[O:15])[CH2:9]2)[CH:7]=1.C([O-])(=O)C.[NH4+:21]>C(O)C>[NH2:21][CH:12]1[CH2:13][CH:8]([C:6]2[CH:7]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[F:16])[CH2:9][C:10](=[O:15])[CH2:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 183175245-(5-Chloro-2-fluorophenyl)cyclohexane-1,3-dione

생성물 1

HCID 183173031-Amino-5-(5-chloro-2-fluorophenyl)cyclohexan-3-one수율 72.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 5-(5-chloro-2-fluorophenyl)cyclohexane-1,3-dione (2 g) and ammonium acetate (1.9 g) in ethanol (15 ml) was refluxed for 15 hours. The reaction solution was concentrated under reduced pressure, and to the residue were added water (30 ml) and ethyl acetate (150 ml). The mixture was shaken, and the separated upper layer was washed with water and concentrated under reduced pressure. The residue was washed with ethyl acetate and dried to give 1-amino-5-(5-chloro-2-fluorophenyl)cyclohexan-3-one (1.45 g) as yellow crystals.

후처리

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionto the residue were added water (30 ml) and ethyl acetate (150 ml)
  3. washthe separated upper layer was washed with water
  4. concentrationconcentrated under reduced pressure
  5. washThe residue was washed with ethyl acetate
  6. customdried

출처 및 근거

ORD 기록
ord-72ae725777ab457b997cae867f223b74
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06350749B1

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