反应详情

温度

-78 °C

A solution of dimethyl methylphosphonate (35.0 ml) in THF (300 ml) was cooled to -78° C., to which n-butyllithium (1.6-M, 196 ml) was added dropwise. After stirring at -78° C. for one hour, a solution of ethyl 2,2-dimethylcaproate (27 g) in dry THF was added. The reaction solution was stirred at -78° C. for one hour, and then at room temperature for additional 2 hours. The reaction solution was cooled to 0° C. and acetic acid (18 ml) was added thereto. The crude product obtained after the conventional work-up was distilled under reduced pressure and the resulting fraction (>130° C.) was chromatographed to give dimethyl (3,3-dimethyl-2-oxoheptyl)phosphonate. Yield, 9.72 g (26%)

1. additionwas added dropwise
2. stirringThe reaction solution was stirred at -78° C. for one hour
3. waitat room temperature for additional 2 hours
4. temperatureThe reaction solution was cooled to 0° C.
5. customThe crude product obtained after the conventional work-up
6. distillationwas distilled under reduced pressure
7. customthe resulting fraction (>130° C.) was chromatographed