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Methyl iodide → HCID 67326839, Verbindung

HRID 1500749
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1500749
[H-].[Na+].[C:3]([C:5]1[CH:10]=[CH:9][N:8]2[N:11]=[CH:12][C:13]([C:14]3[N:19]=[C:18]([NH:20][C@@H:21]4[CH2:26][CH2:25][CH2:24][N:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:22]4)[CH:17]=[CH:16][N:15]=3)=[C:7]2[CH:6]=1)#[N:4].[CH3:34]I>CN(C)C=O>[C:3]([C:5]1[CH:10]=[CH:9][N:8]2[N:11]=[CH:12][C:13]([C:14]3[N:19]=[C:18]([N:20]([CH3:34])[C@@H:21]4[CH2:26][CH2:25][CH2:24][N:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:22]4)[CH:17]=[CH:16][N:15]=3)=[C:7]2[CH:6]=1)#[N:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 67326745HCID 67326745, Verbindung

Produkt 1

HCID 67326839HCID 67326839, VerbindungAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Sodium hydride (60% dispersion in mineral oil, 102 mg, 2.55 mmol) was added to a cooled (0° C.) solution of tert-butyl (3R)-3-{[2-(5-cyanopyrazolo[1,5-a]pyridin-3-yl) pyrimidin-4-yl]amino}piperidine-1-carboxylate (Preparation 7a, 0.83 g, 1.98 mmol) in NIP-dimethylformamide (5 mL) and the reaction mixture was stirred at the same temperature for 30 minutes. Methyl iodide (0.135 mL, 2.17 mmol) was then added and the reaction mixture was stirred at room temperature for 2 hours. The solvent was concentrated in vacuo and the residue was partitioned between water and ethyl acetate. The organic layer was separated, washed with water and brine, dried (MgSO4) and the solvent was evaporated to give the title compound (0.39 g, 80%) as a beige solid.

Aufarbeitung

  1. stirringthe reaction mixture was stirred at room temperature for 2 hours
  2. concentrationThe solvent was concentrated in vacuo
  3. customthe residue was partitioned between water and ethyl acetate
  4. customThe organic layer was separated
  5. washwashed with water and brine
  6. dry with materialdried (MgSO4)
  7. customthe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-b8b01be62e634357ae65c309a0a7948c
Quelldatensatz
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09206183B2

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