Potassium Carbonate → HCID 58901904, 화합물

HRID 459801노트

반응식

HRID 459801 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 58901904HCID 58901904, 화합물수율 32.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0b3019801719495bb584356e648369cd
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07196087B2

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