反应详情

Boron trifluoride dimethyl sulfide complex (70 mL) was added into a mixture of N-(4 -chloro-2,5-dimethoxyphenyl)-3-fluoro-4-methoxybenzamide (1.75 g, 5.15 mmol) and CH2Cl2 (35 mL). After stirring for 20 h, the solvent and the excess reagent were evaporated under a nitrogen stream in the hood. The residue was taken in a mixture of ice and HCl (1N) and extracted with EtOAc. The organic layer was washed with HCl (1N) and dried over MgSO4. Evaporation and purification by flash chromatography (CH2Cl2/hexanes/EtOAc 5/3/2, and AcOH 10 mL per 1 liter of the eluting solvent) gave a white solid (1.4 g, 91% yield, m.p. 254–256° C.); MS m/e 296 (M−H)+.

1. customthe solvent and the excess reagent were evaporated under a nitrogen stream in the hood
2. additionThe residue was taken in a mixture of ice and HCl (1N)
3. extractionextracted with EtOAc
4. washThe organic layer was washed with HCl (1N)
5. dry with materialdried over MgSO4
6. customEvaporation and purification by flash chromatography (CH2Cl2/hexanes/EtOAc 5/3/2, and AcOH 10 mL per 1 liter of the eluting solvent)