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

HRID 1398081

反応式

HRID 1398081 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-0b6c5cac907949109adf83a4e2b30cfe
出典データセット
uspto-grants-2014_12
特許番号
US08901315B2

関連ノート

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