Methyl iodide → 1-Methyl-5-[(1-methyl-1H-pyrazol-4-yl)methyl]-2-(nitroamino)-4(1H)-pyrimidinone

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Reaktionsgleichung

[CH3:1][N:2]1[CH:6]=[C:5]([CH2:7][C:8]2[C:9](=[O:18])[N:10]=[C:11]([NH:14][N+:15]([O-:17])=[O:16])[NH:12][CH:13]=2)[CH:4]=[N:3]1.[CH3:19]CN(C(C)C)C(C)C.CI>C(Cl)(Cl)Cl>[CH3:19][N:12]1[CH:13]=[C:8]([CH2:7][C:5]2[CH:4]=[N:3][N:2]([CH3:1])[CH:6]=2)[C:9](=[O:18])[N:10]=[C:11]1[NH:14][N+:15]([O-:17])=[O:16]

Komponenten

Reaktionsbedingungen

Temperatur: 23 °C

Versuchsvorschrift

A solution of 5-[(1-methyl-1H-pyrazol-4-yl)methyl]-2-(nitroamino)-4(1H)-pyrimidinone (500 mg, 1.998 mmol) and DIPEA (1.745 mL, 9.99 mmol) in chloroform (5 mL) was mixed with methyl iodide (0.150 mL, 2.398 mmol). The reaction mixture was stirred at 23° C. overnight. Purification via HPLC then afforded the title compound (103 mg, 19.51% yield). LCMS: rt=1.46 min, [M+H+]=265.1

Aufarbeitung

customPurification via HPLC

Quellen und Nachweise

ORD-Eintrag: ord-3cf282c6ff2e47edbf1ed065b409c3a0
Quelldatensatz: uspto-grants-2014_01
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08637536B2

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