反应详情

温度

-78 °C

To a solution of trimethylsilyltrifluoromethanesulfonate (0.034 mL) in dry dichloromethane (5 mL) was added 1,2-bis(trimethylsiloxy)ethane (4.55 mL) followed by methyl 3-oxocyclohexanecarboxylate (2.9 g). The reaction mixture was stirred for 3 hours at −78° C. The reaction mixture was quenched with dry pyridine (0.5 mL), poured into saturated aqueous NaHCO3, and extracted with ether. The ether layer was dried over Na2CO3/Na2SO4. The reaction mixture was concentrated and purified by flash chromatography on silica with 5 to 30% ethyl acetate in hexanes to provide the title compound.

1. customThe reaction mixture was quenched with dry pyridine (0.5 mL)
2. additionpoured into saturated aqueous NaHCO3
3. extractionextracted with ether
4. dry with materialThe ether layer was dried over Na2CO3/Na2SO4
5. concentrationThe reaction mixture was concentrated
6. custompurified by flash chromatography on silica with 5 to 30% ethyl acetate in hexanes