Methanol → HCID 178491832、化合物

HRID 2095642ノート

反応式

HRID 2095642 の反応式
[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[CH:23]=[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[CH:23]=[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]

参加物

5

反応物 4

HCID 887MethanolHCID 962WaterHCID 3939Lithium HydroxideHCID 178472397HCID 178472397、化合物

生成物 1

HCID 178491832HCID 178491832、化合物

実験手順

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}-5-methyl-1H-pyrazol-1-yl)cyclohexanecarboxylate (20.0 mg, 0.0371 mmol) in MeOH (3 mL, 70 mmol) was added lithium hydroxide (4.44 mg, 0.186 mmol) and H2O (1 mL, 60 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 (pH=2). The organic layer was concentrated in vacuo to afford the title compound as a white solid. MS (ES+): m/z=511.19/513.19 (100/50) [MH+]. HPLC: tR=1.44 min (polar—3 min, UPLC-ACQUITY).

後処理

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

出典と根拠

ORDレコード
ord-09dddfbe5fa047d49d48a6b8d6e87c04
出典データセット
uspto-grants-2013_05
特許番号
US08445510B2

反応ノート

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