3-[6-Chloro-2-(4-nitro-phenyl)-pyrimidin-4-yl]-8-oxa-3-aza-bicyclo[3.2.1]octane → Isopropyl-[2-(4-nitro-phenyl)-6-(8-oxa-3-aza-bicyclo[3.2.1]oct-3-yl)-pyrimidin-4-yl]-amine

HRID 75415

Reaktionsgleichung

Cl[C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=2)[N:5]=[C:4]([N:17]2[CH2:23][CH:22]3[O:24][CH:19]([CH2:20][CH2:21]3)[CH2:18]2)[CH:3]=1>C(N)(C)C>[CH:11]([NH:14][C:2]1[CH:3]=[C:4]([N:17]2[CH2:23][CH:22]3[O:24][CH:19]([CH2:20][CH2:21]3)[CH2:18]2)[N:5]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=2)[N:7]=1)([CH3:12])[CH3:10]

Komponenten

Reaktionsbedingungen

Temperatur: 140 °C

Versuchsvorschrift

In a 2-5 mL microwave vial was placed 3-(6-chloro-2-(4-nitrophenyl)pyrimidin-4-yl)-8-oxa-3-azabicyclo[3.2.1]octane (13, 70 mg, 0.202 mmol) in iPrNH2 (4 ml) to give a yellow suspension. The reaction was heated under microwave irradiation at 140° C. for 90 min. The mixture was concentrated, dissolved in dichloromethane and washed with sat NaHCO3. The organic phase was dried over MgSO4, filtered and concentrated to give 74 mg of the title compound as a yellow solid (99%).

Aufarbeitung

customto give a yellow suspension
concentrationThe mixture was concentrated
dissolutiondissolved in dichloromethane
washwashed
dry with materialThe organic phase was dried over MgSO4
filtrationfiltered
concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag: ord-fbe7ae7ed2ba4f29b4669ac13aad8e01
Quelldatensatz: uspto-grants-2014_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08835429B2

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