Methanol → HCID 178491826, 화합물

HRID 2095650노트

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HRID 2095650 반응식
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([O:9][CH3:10])[C:3]=1[C@H:11]([C:13]1[C:21]2[C:16](=[N:17][CH:18]=[C:19]([C:22]3[C:23]([CH3:39])=[N:24][N:25]([C@H:28]4[CH2:33][CH2:32][C@H:31]([C:34]([O:36]CC)=[O:35])[CH2:30][CH2:29]4)[C:26]=3[CH3:27])[CH:20]=2)[NH:15][CH:14]=1)[CH3:12].CO.[OH-].[Li+].O>>[Cl:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([O:9][CH3:10])[C:3]=1[C@H:11]([C:13]1[C:21]2[C:16](=[N:17][CH:18]=[C:19]([C:22]3[C:23]([CH3:39])=[N:24][N:25]([C@H:28]4[CH2:33][CH2:32][C@H:31]([C:34]([OH:36])=[O:35])[CH2:30][CH2:29]4)[C:26]=3[CH3:27])[CH:20]=2)[NH:15][CH:14]=1)[CH3:12]

참가 물질

5

반응물 4

HCID 887MethanolHCID 962WaterHCID 3939Lithium HydroxideHCID 178472400HCID 178472400, 화합물

생성물 1

HCID 178491826HCID 178491826, 화합물

실험 절차

A solution of ethyl trans-4-(4-{3-[(1S)-1-(2-chloro-3-fluoro-6-methoxyphenyl)ethyl]-1H-pyrrolo[2,3-b]pyridin-5-yl}-3,5-dimethyl-1H-pyrazol-1-yl)cyclohexanecarboxylate (9.00 mg, 0.0163 mmol) in MeOH (1 mL, 30 mmol) was added lithium hydroxide (1.95 mg, 0.0814 mmol) and H2O (0.4 mL, 20 mmol). The mixture was stirred at rt for 2 h. The organic solvent was removed in vacuo, and the material was extracted with DCM and water at pH 2. The organic layer was concentrated in vacuo to afford the title compound as a white solid. MS (ES+): m/z=525.21/527.21 (100/50) [MH+]. HPLC: tR=1.45 min (polar—3 min, UPLC-ACQUITY).

후처리

  1. customThe organic solvent was removed in vacuo
  2. extractionthe material was extracted with DCM and water at pH 2
  3. concentrationThe organic layer was concentrated in vacuo

출처 및 근거

ORD 기록
ord-70c2fcf4758941899aa191050bf3f82b
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445510B2

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