Dimethyl (2,5-dimethylbenzoyl)phosphonate → HCID 13841522, Verbindung
Reaktionsgleichung
[CH3:1][C:2]1[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][C:3]=1[C:4]([P:6](=[O:11])([O:9][CH3:10])[O:7][CH3:8])=[O:5].[P:17]([O-:22])([O:20][CH3:21])[O:18][CH3:19]>>[P:17]([O:5][CH:4]([P:6]([O:9][CH3:10])([O:7][CH3:8])=[O:11])[C:3]1[CH:12]=[C:13]([CH3:16])[CH:14]=[CH:15][C:2]=1[CH3:1])([O:20][CH3:21])([O:18][CH3:19])=[O:22]Komponenten
3
Versuchsvorschrift
A mixture of 5.0 g (20.7 mmol) dimethyl 2,5-dimethylbenzoylphosphonate and 2.73 g (24.8 mmol) dimethyl phosphite was heated at 110° for 5 h. The excess of dimethyl phosphite and the unreacted benzoylphosphonate were removed under vacuum. The yellow viscous residue was then purified by column chromatography with chloroform as the eluent. Dimethyl α-(dimethoxyphosphinyl)2,5-dimethylbenzyl phosphate was obtained as a white oil (2.06 g, 29%); GLC and TLC analysis showed the compound to be pure.
Aufarbeitung
- temperaturewas heated at 110° for 5 h
- customThe excess of dimethyl phosphite and the unreacted benzoylphosphonate were removed under vacuum
- customThe yellow viscous residue was then purified by column chromatography with chloroform as the eluent