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Lithium Hydroxide → HCID 178525787、化合物

HRID 931290
ノート
印刷プレビュー

反応式

HRID 931290 の反応式
[OH-].[Li+].[Cl:3][C:4]1[CH:5]=[N:6][N:7]([C:9]2([C:12]3[NH:31][C:15]4=[N:16][C:17]([N:20]5[CH2:25][CH2:24][CH2:23][C@@H:22]([C:26]([O:28]CC)=[O:27])[CH2:21]5)=[CH:18][CH:19]=[C:14]4[N:13]=3)[CH2:11][CH2:10]2)[CH:8]=1>O1CCCC1.O>[Cl:3][C:4]1[CH:5]=[N:6][N:7]([C:9]2([C:12]3[NH:31][C:15]4=[N:16][C:17]([N:20]5[CH2:25][CH2:24][CH2:23][C@@H:22]([C:26]([OH:28])=[O:27])[CH2:21]5)=[CH:18][CH:19]=[C:14]4[N:13]=3)[CH2:10][CH2:11]2)[CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 178472506(R)-ethyl 1-(2-(1-(4-chloro-1H-pyrazol-1-yl)cyclopropyl)-3H-imidazo[4,5-b]pyridin-5-yl)piperidine-3-carboxylate

生成物 1

HCID 178525787HCID 178525787、化合物収率 83.4%

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

Lithium hydroxide (500 mg, 10.20 mmol) was added to a solution of (R)-ethyl 1-(2-(1-(4-chloro-1H-pyrazol-1-yl)cyclopropyl)-3H-imidazo[4,5-b]pyridin-5-yl)piperidine-3-carboxylate (900 mg, 2.17 mmol) in tetrahydrofuran/water (1:1, 10 mL) at room temperature. The reaction mixture was stirred for 3 h. The solvent was removed under reduced pressure and to the residue was added water. The pH of the mixture was adjusted to 6 using an aqueous solution of hydrochloric acid (1N). The mixture was extracted with ethyl acetate and the organics were dried over sodium sulfate, filtered and concentrated to afford (R)-1-(2-(1-(4-chloro-1H-pyrazol-1-yl)cyclopropyl)-3H-imidazo[4,5-b]pyridin-5-yl)piperidine-3-carboxylic acid (700 mg). MS (ES+) (M+H) 387.1; LCMS retention time 1.971 min (Method N1).

後処理

  1. customThe solvent was removed under reduced pressure and to the residue
  2. additionwas added water
  3. extractionThe mixture was extracted with ethyl acetate
  4. dry with materialthe organics were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-57b01088bfdd43a0bb412195773a9e53
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296745B2

反応ノート

読み込み中…

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