反应详情

温度

0 °C

[4-Methyl-3-(tetrahydro-pyran-2-yloxymethyl)-pyridin-2-yl]-methanol (138 mg. 0.58 mmol) was dissolved in DCM (5 mL) and cooled to 0° C. NEt3 (324 μL. 2.33 mmol) and methanesulfonyl chloride (90 μL. 1.16 mmol) were added and the reaction mixture was stirred for 1 h at 0° C. After removal of the solvents in vacuo the residue was dissolved in DMF (10 mL) and CsCO3 (570 mg. 1.75 mmol) and 3-trifluoromethyl-pyridin-2-ol (142 mg. 0.87 mmol) were added. After stirring for 2 h at RT the solvent was removed in vacuo and the residue was partioned between water (20 mL) and DCM (20 mL) extracted with DCM (3×20 mL) and the combined organic fractions were dried over Na2SO4 filtered and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (elution with hexane/EtOAc 2:1→1:1) to give the title compound. MS (m/z): 382.9 [M+H+].

1. customAfter removal of the solvents in vacuo the residue
2. dissolutionwas dissolved in DMF (10 mL)
3. stirringAfter stirring for 2 h at RT the solvent
4. customwas removed in vacuo
5. extractionextracted with DCM (3×20 mL)
6. dry with materialthe combined organic fractions were dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe residue was purified by flash chromatography on silica gel (elution with hexane/EtOAc 2:1→1:1)