Potassium Carbonate → HCID 58901904、化合物

HRID 459801ノート

反応式

HRID 459801 の反応式
F[C:2]1[C:9]([F:10])=[CH:8][CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:5].C(=O)([O-])[O-].[K+].[K+].[C:18]([O:22][C:23]([N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1)=[O:24])([CH3:21])([CH3:20])[CH3:19]>CN(C=O)C>[C:18]([O:22][C:23]([N:25]1[CH2:30][CH2:29][N:28]([C:2]2[C:9]([F:10])=[CH:8][CH:7]=[C:6]([F:11])[C:3]=2[C:4]#[N:5])[CH2:27][CH2:26]1)=[O:24])([CH3:21])([CH3:19])[CH3:20]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 1456222,3,6-Trifluorobenzonitrile

生成物 1

HCID 58901904HCID 58901904、化合物収率 32.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 1.0 g (6.36 mmol)of 2,3,6-trifluorobenzonitrile dissolved in 10 mL DMF was added 1.05 g (1.2 eq., 7.63 mmol) potassium carbonate and 1.18 g (1 eq., 6.36 mmol) piperazine-1-carboxylic acid tert-butyl ester. The mixture was stirred 30 minutes to completion, partitioned between ethyl acetate and water, dried over magnesium sulfate and concentrated under reduced pressure. Column chromatography, eluting with ethyl acetate/hexanes provided 665 mg of 4-(2-cyano-3,6-difluoro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester.

後処理

  1. custompartitioned between ethyl acetate and water
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. washColumn chromatography, eluting with ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-0b3019801719495bb584356e648369cd
出典データセット
uspto-grants-2007_03
特許番号
US07196087B2

反応ノート

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