反应详情

温度

-78 °C

A solution of ii (0.30 g, 1.0 mmol) in THF (10 mL) was cooled to −78° C. followed by dropwise addition of LDA (1.60 M in THF, 1.88 mL, 3.0 mmol) at −78° C. The mixture was stirred at −78° C. for 30 min followed by addition of methyl iodide (0.311 mL, 5.0 mmol) at −78° C. The temperature of the reaction mass was slowly raised up to RT and left to stir overnight. The reaction was cooled to 0° C. and quenched by dropwise addition of saturated NH4Cl solution (30 mL). The reaction was extracted with EtOAc (3×50 mL). The combined organics were washed with brine, dried (Na2SO4), filtered and concentrated in vacuo to obtain iii (0.30 g, 97%). MS 316.12 [M+H]+.

1. temperatureThe temperature of the reaction mass was slowly raised up to RT
2. waitleft
3. stirringto stir overnight
4. temperatureThe reaction was cooled to 0° C.
5. customquenched by dropwise addition of saturated NH4Cl solution (30 mL)
6. extractionThe reaction was extracted with EtOAc (3×50 mL)
7. washThe combined organics were washed with brine
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated in vacuo