反应详情

温度

-78 °C

Chloro-3-methoxy-1-trityl-1H-pyrazolo[4,3-c]pyridine-4-carbaldehyde (Intermediate 11B, 535 mg, 1.2 mmol) was dissolved in THF (8 ml) cooled to −78° C. and charged with methylmagnesium bromide (3M, 0.786 ml, 2.357 mmol). The reaction was allowed to stir for 1 hr, eventually reaching 0° C. The reaction was slowly quenched with saturated ammonium chloride (3 mL) and partioned between EtOAc 2×10 mL, washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. The residue was then loaded onto silica gel and purified by MPLC 0-25% EtOAc/hexanes to provide 1-(6-chloro-3-methoxy-1-trityl-1H-pyrazolo[4,3-c]pyridin-4-yl)ethanol (38B). MS: [M+H]+ m/z 470.

1. customeventually reaching 0° C
2. customThe reaction was slowly quenched with saturated ammonium chloride (3 mL)
3. washwashed with brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. custompurified by MPLC 0-25% EtOAc/hexanes