反应详情

4 g of diethyl 2-methylbenzylphosphonate were added to a solution of 12 g of KMnO4 and 4 g of Na2CO3 in 300 ml of water and the mixture was boiled under reflux for 24 hours. It was acidified with 15 ml of concentrated H2SO4 and extracted five times with 300 ml of ether each time. The organic phase was dried over MgSO4, the solvent was evaporated off on a rotary evaporator and the residue was chromatographed over silica gel (CH2Cl2 /methanol/triethylamine 9/1/0.1).

1. temperatureunder reflux for 24 hours
2. extractionextracted five times with 300 ml of ether each time
3. dry with materialThe organic phase was dried over MgSO4
4. customthe solvent was evaporated off on a rotary evaporator
5. customthe residue was chromatographed over silica gel (CH2Cl2 /methanol/triethylamine 9/1/0.1)