Potassium Carbonate → 1-(2-Fluoro-4-nitrophenyl)piperidin-4-ol

HRID 1398081

반응식

HRID 1398081 반응식
[F:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1F.C(=O)([O-])[O-].[K+].[K+].[OH:18][CH:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1>CN(C)C=O.C(Cl)(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1[N:22]1[CH2:23][CH2:24][CH:19]([OH:18])[CH2:20][CH2:21]1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 79341Piperidin-4-olHCID 1230531,2-Difluoro-4-nitrobenzene

생성물 1

HCID 265982211-(2-Fluoro-4-nitrophenyl)piperidin-4-ol수율 43%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

To a solution of 4.77 g (30.0 mmol) of 3,4-difluoronitrobenzene in 100 mL of N,N-dimethylformamide were added 5.33 g (40.0 mmol) of potassium carbonate and 3.03 g (30.0 mmol) of 4-hydroxypiperidine and the mixture was stirred for 1 hour at 120° C. After the reaction mixture was cooled to room temperature, the reaction mixture was diluted with chloroform and insoluble substances were removed off by filtration. The filtrate was condensed and the residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=1.5/1) to give 3.1 g (43%) of the title compound.

후처리

  1. temperatureAfter the reaction mixture was cooled to room temperature
  2. customwere removed off by filtration
  3. customcondensed
  4. customthe residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=1.5/1)

출처 및 근거

ORD 기록
ord-0b6c5cac907949109adf83a4e2b30cfe
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08901315B2

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