反应详情

温度

-78 °C

Dimethyl methylphosphonate (14.88 g) is dissolved in dry tetrahydrofuran (THF, 34 ml) under a nitrogen atmosphere. The solution is cooled to -78° C. Butyllithium (7.68 g, 52 ml of 2.3 molar solution, 3 equiv.) is added very slowly during 1 hour. The mixture is stirred at -78° C for 15 minutes. A solution of 2,2-dimethylhexanoic acid methyl ester (6.32 g) in dry THF (16 ml) is added to the cold solution over a period of 1 hour. The mixture is stirred for 30 minutes and then allowed to warm up to room temperature. The reaction mixture is diluted with ether. Dilute (10%) hydrochloric acid (30 ml) is added and the reaction mixture shaken well. The organic phase is separated and washed several times with water, dried (MgSO4) and the solvent removed. The residue is distilled under reduced pressure to give the title compound, b.p. 110° - 120° C/0.1mm, γmaxfilm 1700, 1250, 1020 cm-1.

1. stirringThe mixture is stirred for 30 minutes
2. temperatureto warm up to room temperature
3. additionis added
4. stirringthe reaction mixture shaken well
5. customThe organic phase is separated
6. washwashed several times with water
7. dry with materialdried (MgSO4)
8. customthe solvent removed
9. distillationThe residue is distilled under reduced pressure