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Lithium Hydroxide → HCID 60205665, Verbindung

HRID 2203976
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2203976
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
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Komponenten

10

Edukt 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

Produkt 1

HCID 60205665
HCID 60205665, Verbindung
Ausbeute 61,8 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 962WaterLösungsmittel2×HCID 6342AcetonitrileLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 13387N-methyl-2-pyrrolidoneLösungsmittel2×

Versuchsvorschrift

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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-95b6013c9b5c4eb491919f44f11dc717
Quelldatensatz
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09365568B2

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