反应详情

Triethylamine (1.7 mL, 12 mmol) was added under ice cooling to a mixture of (6-methyl-1,3-dihydro-2-benzofuran-5-yl)methanol described in Production Example 1-5 (1.0 g, 6.1 mmol) and dichloromethane (10 mL), followed by the addition of methanesulfonyl chloride (470 μL, 6.1 mmol) at that temperature. The reaction mixture was stirred for 3 hours at room temperature. Water was added to the reaction mixture, which was then extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:10) to give the title compound (680 mg, 61% yield).

1. extractionwas then extracted with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled away under reduced pressure
5. customThe residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:10)