反应详情

温度

115 °C

A solution of N′-hydroxy-3-(trifluoromethyl)benzenecarboximidamide (2.1 g) in pyridine (20 mL) was cooled in an ice bath, and the compound (2.3 g) obtained in Example 115c was added. The reaction mixture was stirred overnight with heating at 110-120° C. The mixture was poured into water, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was separated, washed successively with 1N hydrochloric acid and saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate) to give the title compound (0.38 g) as a solid.

1. extractionthe mixture was extracted with ethyl acetate
2. customThe ethyl acetate layer was separated
3. washwashed successively with 1N hydrochloric acid and saturated brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate)