反应详情

温度

150 °C

7-Fluoro-2-[3-(hydroxymethyl)azetidin-1-yl]-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-192) (220 mg, 0.37 mmol) was dissolved in dimethyl sulfoxide (5 ml), then triethylamine (166 μl, 1.19 mmol) and (3S)-3-(dimethylamino)pyrrolidine (159 μl, 1.25 mmol) were added, followed by stirring in a sealed tube at 150° C. for 19 hours. After cooling, concentration under reduced pressure, dilution with methylene chloride and washing with water, the organic layer was dried over anhydrous magnesium sulfate, then the solvent was evaporated away under reduced pressure. The resulting residue was subjected to preparative silica gel column chromatography. The eluate with chloroform/methanol (10:1, v/v) gave the entitled compound (208 mg, 74%) as a white amorphous substance.

1. temperatureAfter cooling
2. concentrationconcentration under reduced pressure, dilution with methylene chloride
3. washwashing with water
4. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
5. customthe solvent was evaporated away under reduced pressure