反应详情

温度

-65 °C

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of [2-(2-dihydroxymethyl-oxazol-4-ylmethyl)-2H-[1,2,3]triazol-4-yl]-carbamic acid 2-chloro-benzyl ester (19 mg, 0.05 mmol) in THF (1.0 mL) was treated at −65° C. with methylmagnesium bromide (0.15 mL of a 1M solution in THF, 0.15 mmol). The reaction mixture was then stirred at −65° C. for 1 h. The reaction mixture was then slowly warmed to rt and stirred at this temperature for 45 min. Sat. aq. NH4Cl was then added and the aq. layer was extracted with EA (3×10 mL). The combined org. extracts were dried over Na2SO4, filtered, and the solvents were removed under reduced pressure. The residue was purified by FC (EA) to give the title compound as a yellow oil. TLC: rf (EA)=0.30. LC-MS-conditions 02: tR=0.89 min, [M+H]+=378.30.

1. temperatureThe reaction mixture was then slowly warmed to rt
2. stirringstirred at this temperature for 45 min
3. extractionthe aq. layer was extracted with EA (3×10 mL)
4. dry with materialextracts were dried over Na2SO4
5. filtrationfiltered
6. customthe solvents were removed under reduced pressure
7. customThe residue was purified by FC (EA)