反应详情

1-(5,6-Dichloro-1H-benzoimidazol-2-yl)-2,2,2-trifluoro-ethanone (0.3005 g; 1.062 mmoles) and hydroxylamine hydrochloride (0.2389 g, 3.438 mmoles) were suspended in pyridine (3 mL) and ethanol (3 mL), then heated to 70° C. for 3 hrs. The reaction mixture was cooled to room temperature, water was water (50 mL) and the reaction mixture was then extracted with ethyl acetate (3×40 ml). The extracts were combined then washed with water (20 mL), brine (30 mL) and dried over Na2SO4. The filtrate was concentrated in vacuo and purified by column chromatography (SiO2; 30% ethyl acetate/CH2Cl2) to yield the title compound as an off-white solid, as a mixture of oxime E and Z isomers.

1. extractionthe reaction mixture was then extracted with ethyl acetate (3×40 ml)
2. washThe extracts were combined then washed with water (20 mL), brine (30 mL)
3. dry with materialdried over Na2SO4
4. concentrationThe filtrate was concentrated in vacuo
5. custompurified by column chromatography (SiO2; 30% ethyl acetate/CH2Cl2)