Water → 1-(4-bromo-2,5-difluoro-phenyl)-piperidin-4-one O-[1-(5-ethyl-pyrimidin-2-yl)-piperidin-4-yl]-oxime

HRID 2066903노트

반응식

HRID 2066903 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([O:7][N:8]=[C:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:20]=[C:19]([F:21])[C:18]([Br:22])=[CH:17][C:16]=3[F:23])[CH2:11][CH2:10]2)[CH2:3][CH2:2]1.Cl[C:25]1[N:30]=[CH:29][C:28]([CH2:31][CH3:32])=[CH:27][N:26]=1.C(N(C(C)C)CC)(C)C.O>CS(C)=O.CCOC(C)=O>[CH2:31]([C:28]1[CH:27]=[N:26][C:25]([N:1]2[CH2:6][CH2:5][CH:4]([O:7][N:8]=[C:9]3[CH2:14][CH2:13][N:12]([C:15]4[CH:20]=[C:19]([F:21])[C:18]([Br:22])=[CH:17][C:16]=4[F:23])[CH2:11][CH2:10]3)[CH2:3][CH2:2]2)=[N:30][CH:29]=1)[CH3:32]

참가 물질

7

반응물 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 35727632-Chloro-5-ethylpyrimidineHCID 866550281-(4-bromo-2,5-difluoro-phenyl)-piperidin-4-one O-piperidin-4-yl-oxime

생성물 1

HCID 866550291-(4-bromo-2,5-difluoro-phenyl)-piperidin-4-one O-[1-(5-ethyl-pyrimidin-2-yl)-piperidin-4-yl]-oxime

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 8857Ethyl Acetate용매

실험 절차

Compound 77b and 2-chloro-5-ethyl-pyrimidine (300 mg) were heated with diisopropylethylamine (300 mg) in DMSO at 130° C. for 0.5 h. Water and EtOAc were added and the organic phase separated, dried over MgSO4 and concentrated. The mixture was purified by chromatography on silica gel eluting with EtOAc/Hexane to give 1-(4-bromo-2,5-difluoro-phenyl)-piperidin-4-one O-[1-(5-ethyl-pyrimidin-2-yl)-piperidin-4-yl]-oxime 77c (170 mg).

후처리

  1. customthe organic phase separated
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated
  4. customThe mixture was purified by chromatography on silica gel eluting with EtOAc/Hexane

출처 및 근거

ORD 기록
ord-a5d3ba83d9f64223a822d77c5a7dccc7
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293729B2

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