反应详情

温度

-78 °C

Under a nitrogen atmosphere Compound 11 (0.15 g, 0.43 mmol) was dissolved in THF (2 mL) and N-methoxy-N-methylbenzamide (0.14 g, 0.86 mmol) was added. The resulting solution was cooled to −78° C. and tert-Butyl lithium (1.7M in THF, 1.02 mL, 1.73 mmol) was added dropwise. The resulting mixture was stirred and cooled for 1 h and quenched with NH4Cl saturated solution. The solid was removed by filtration and the filtrate was concentrated, acidified to pH 6 with 5% TFA and extracted with 20% i-PrOH/DCM. The organic layer was concentrated, diluted with DCM, washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to give product 25A (0.072 g, 45%). LCMS (+ESI) m/z 372.1 [M+H]+.

1. temperaturecooled for 1 h
2. customquenched with NH4Cl saturated solution
3. customThe solid was removed by filtration
4. concentrationthe filtrate was concentrated
5. extractionextracted with 20% i-PrOH/DCM
6. concentrationThe organic layer was concentrated
7. additiondiluted with DCM
8. washwashed with brine
9. dry with materialdried over anhydrous Na2SO4
10. filtrationfiltered
11. concentrationconcentrated