반응 #162704

반응 방정식

2-fluoro-4-formylbenzonitrile

4,5-dimethyl benzene-1,2-diamine

p-toluenesulfonic acid

→

compound 3

수율 68.0%

4-(5,6-dimethyl-1H-benzo[d]imidazol-2-yl)-2-fluorobenzo-nitrile

수율 68.0%

용매

ethanol

반응 조건

후처리

1. 1
   온도reflux for 2 hours
2. 2
   농축concentrated by rotor evaporation
3. 3
   기타The crude material was purified through column chromatography with 40% ethyl acetate in hexane

실험 절차

To a solution of 2-fluoro-4-formylbenzonitrile 1 (100 mg, 0.7 mmol) and 4,5-dimethyl benzene-1,2-diamine 2 (109 mg, 0.8 mmol) in ethanol (10 ml) was added a catalytic amount of p-toluenesulfonic acid (0.5 mg, 0.5 mmol). The mixture was stirred reflux for 2 hours and concentrated by rotor evaporation. The crude material was purified through column chromatography with 40% ethyl acetate in hexane to yield compound 3 as white solid (68% yield, 121 mg, confirmed by LCMS: 266.20).

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