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Lithium Hydroxide → HCID 60205665、化合物

HRID 875896
ノート
印刷プレビュー

反応式

HRID 875896 の反応式
CCN(C(C)C)C(C)C.[CH3:10][O:11][C@H:12]([CH3:16])[C:13](O)=[O:14].C1N(P([Cl:31])(N2C(=O)OCC2)=O)C(=O)OC1.[NH2:32][C:33]1[C:41]2[C:36](=[N:37][CH:38]=[C:39]([Cl:56])[C:40]=2[N:42]2[CH2:47][CH2:46][CH2:45][C@@H:44]([NH:48]C(=O)OC(C)(C)C)[CH2:43]2)[NH:35][CH:34]=1.[Li+].[OH-]>CN1C(=O)CCC1.C(#N)C.O.C(Cl)Cl>[ClH:31].[NH2:48][C@@H:44]1[CH2:45][CH2:46][CH2:47][N:42]([C:40]2[C:39]([Cl:56])=[CH:38][N:37]=[C:36]3[NH:35][CH:34]=[C:33]([NH:32][C:13](=[O:14])[C@H:12]([O:11][CH3:10])[CH3:16])[C:41]=23)[CH2:43]1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 3939Lithium HydroxideHCID 81531DiisopropylethylamineHCID 152842Bis(2-oxo-3-oxazolidinyl)phosphinic chlorideHCID 2733584(2R)-2-methoxypropanoic acidHCID 67045610(R)-tert-butyl 1-(3-amino-5-chloro-1H-pyrrolo[2,3-b]pyridin-4-yl)piperidin-3-ylcarbamate

生成物 1

HCID 60205665HCID 60205665、化合物
収率 61.8%

試薬・触媒・溶媒 4

HCID 962Water溶媒2 回HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒HCID 13387N-methyl-2-pyrrolidone溶媒2 回

実験手順

NMP (4 mL), DIEA (2.47 g, 19.1 mmol), (R)-2-methoxypropanoic acid (1.42 g, 13.7 mmol), and BOP-Cl (3.48 g, 13.7 mmol) were added to a solution of crude (R)-tert-butyl 1-(3-amino-5-chloro-1H-pyrrolo[2,3-b]pyridin-4-yl)piperidin-3-ylcarbamate (1.00 g, 2.73 mmol; Example 91, Step A) in NMP (3.3 mL). The reaction was stirred for 30 minutes. 3M LiOH (25 mL) was then added, and the reaction was stirred at room temperature for 18 hours. Water and DCM were added to the reaction mixture, and the layers were separated. The organic layer was dried, filtered, and concentrated. The resulting residue was purified by reverse phase chromatography (Biotage SP4, C-18 40M+, 5-95% water:ACN) to provide (R)—N-(4-((R)-3-aminopiperidin-1-yl)-5-chloro-1H-pyrrolo[2,3-b]pyridin-3-yl)-2-methoxypropanamide hydrochloride (655 mg, 56% yield) as a solid. 1H NMR (400 MHz, D2O) δ 8.03 (s, 1H), 7.50 (s, 1H), 3.99 (q, 1H), 3.58 (m, 1H), 3.46 (m, 1H), 3.37 (s, 3H), 3.29 (m, 1H), 3.15 (m, 1H), 3.00 (m, 1H), 2.09 (m, 1H), 1.80-1.60 (m, 2H), 1.51 (m, 1H), 1.34 (d, 3H). LCMS (APCI+) m/z 352.0 (M+H)+, Retention time=2.28 minutes (Method 3).

後処理

  1. stirringthe reaction was stirred at room temperature for 18 hours
  2. customthe layers were separated
  3. customThe organic layer was dried
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe resulting residue was purified by reverse phase chromatography (Biotage SP4

出典と根拠

ORDレコード
ord-6a61c8e4f0c149869f7f48487f475a6a
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08981085B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート