Water → HCID 66761312, 화합물

HRID 876315노트

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HRID 876315 반응식
[F:1][C:2]([F:26])([F:25])[O:3][C:4]1[CH:9]=[CH:8][C:7]([CH:10]2[CH2:15][NH:14][CH2:13][CH:12]([NH:16][C:17](=[O:24])[C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:11]2)=[CH:6][CH:5]=1.[CH3:27][N:28]1[CH2:33][CH2:32][N:31]([C:34](Cl)=[O:35])[CH2:30][CH2:29]1.C(N(CC)CC)C.O>ClCCl>[CH3:27][N:28]1[CH2:33][CH2:32][N:31]([C:34]([N:14]2[CH2:15][CH:10]([C:7]3[CH:6]=[CH:5][C:4]([O:3][C:2]([F:1])([F:25])[F:26])=[CH:9][CH:8]=3)[CH2:11][CH:12]([NH:16][C:17]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)=[O:24])[CH2:13]2)=[O:35])[CH2:30][CH2:29]1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 30169354-Methyl-1-piperazinecarbonyl chlorideHCID 66701272N-{5-[4-(trifluoromethoxy)phenyl]piperidin-3-yl}benzamide

생성물 1

HCID 66761312HCID 66761312, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

At 0° C., 100 mg (0.27 mmol) of N-{5-[4-(trifluoromethoxy)phenyl]piperidin-3-yl}benzamide were initially charged in 1.5 ml of dichloromethane, and 89 mg (0.55 mmol) of 4-methylpiperazine-1-carbonyl chloride and 58 μl (0.412 mmol) of triethylamine were added. The mixture was slowly warmed to RT overnight. Water was added, and the reaction mixture was extracted. The organic phase was dried over magnesium sulphate and concentrated under reduced pressure. The residue was then purified by preparative HPLC (Reprosil C18, water/acetonitrile gradient). Yield: 104 mg (77% of theory)

후처리

  1. extractionthe reaction mixture was extracted
  2. dry with materialThe organic phase was dried over magnesium sulphate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was then purified by preparative HPLC (Reprosil C18, water/acetonitrile gradient)

출처 및 근거

ORD 기록
ord-1cabfb216ec04ea1acd54e5d828f0ac4
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987248B2

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