Sodium Bicarbonate → HCID 58012362, Verbindung

HRID 1698545Notizen

Reaktionsgleichung

Cl[C:2]1[N:6]([CH3:7])[C:5]2[C:8]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH2:18][CH3:19])=[CH:9][CH:10]=[CH:11][C:4]=2[N:3]=1.[Br:20][C:21]1[CH:27]=[C:26]([CH3:28])[C:24]([NH2:25])=[C:23]([O:29][CH3:30])[CH:22]=1.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[Br:20][C:21]1[CH:27]=[C:26]([CH3:28])[C:24]([NH:25][C:2]2[N:6]([CH3:7])[C:5]3[C:8]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=4[CH2:18][CH3:19])=[CH:9][CH:10]=[CH:11][C:4]=3[N:3]=2)=[C:23]([O:29][CH3:30])[CH:22]=1

Komponenten

Reaktionsbedingungen

Temperatur: 120 °C

Versuchsvorschrift

A mixture of 100 mg (0.369 mmol) of 2-chloro-7-(2-ethylphenyl)-1-methyl-1H-benzimidazole and 239 mg (1.11 mmol) of 4-bromo-2-methoxy-6-methylaniline was stirred at 120° C. for 15 hours. After cooling, the reaction mixture was neutralized by saturated aqueous sodium hydrogen carbonate, followed by addition of ethyl acetate. The resulting crystals were collected by filtration and washed with water and ethyl acetate, and suspended in hot ethyl acetate. After cooling to room temperature, the crystals were collected by filtration and washed with ethyl acetate and a 50% dimethylsulfoxide/methanol mixture to give 90 mg (54%) of the title compound.

Aufarbeitung

temperatureAfter cooling
filtrationThe resulting crystals were collected by filtration
washwashed with water and ethyl acetate
temperatureAfter cooling to room temperature
filtrationthe crystals were collected by filtration
washwashed with ethyl acetate

Quellen und Nachweise

ORD-Eintrag: ord-28918a6c8bc64e0488f7d7a2fd6b6f38
Quelldatensatz: uspto-grants-2012_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08163935B2

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