反应详情

To 94A (2.8 g, 11 mmol) in THF (50 mL) was added n-BuLi (1.6M in hexane, 8.9 mL) at −78° C. After 10 min stirring, trimethyl borate (2.5 mL) was introduced. The mixture was stirred from −78° C. to rt overnight. The reaction was quenched by 1N HCl and extracted with EtOAc. The organic layer was separated and washed with saturated Na2S2O3, brine and dried over MgSO4. Evaporation of solvent gave product 94B (1.66 g, 88% yield) as a white solid. 1H NMR (400 MHz, CDCl3) δ ppm 2.22 (s, 3H) 6.82 (t, J=9.23 Hz, 1H) 7.26 (t, J=7.69 Hz, 1H).

1. stirringThe mixture was stirred from −78° C. to rt overnight
2. customThe reaction was quenched by 1N HCl
3. extractionextracted with EtOAc
4. customThe organic layer was separated
5. washwashed with saturated Na2S2O3, brine
6. dry with materialdried over MgSO4
7. customEvaporation of solvent