反应详情

温度

-30 °C

Methyl magnesium iodide (3M solution in diethyl ether, 0.14 mL, 0.439 mmol, 1.5 eq) was added at −50° C. to a stirred solution of 184a) (130 mg, 0.292 mmol, 1.0 eq) in dry THF (10 mL). The reaction mixture was stirred for 2 h at −30° C., then quenched with ammonium chloride solution, diluted with water (20 mL) and extracted with ethyl acetate (2×20 mL). The combined organic layers were washed with brine, dried over sodium sulfate, and concentrated. The remnant was purified by preparative TLC using ethyl acetate/pet ether (7:3) as eluent. White solid. Yield: 50 mg (37% of theory).

1. customquenched with ammonium chloride solution
2. additiondiluted with water (20 mL)
3. extractionextracted with ethyl acetate (2×20 mL)
4. washThe combined organic layers were washed with brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe remnant was purified by preparative TLC