反応 #5012

反応方程式

H2SO4

diethyl 2-methylbenzylphosphonate

KMnO4

Na2CO3

→

Diethyl 2-carboxybenzylphosphonate

溶媒

water

反応条件

後処理

1. 1
   温度under reflux for 24 hours
2. 2
   抽出extracted five times with 300 ml of ether each time
3. 3
   乾燥The organic phase was dried over MgSO4
4. 4
   その他the solvent was evaporated off on a rotary evaporator
5. 5
   その他the residue was chromatographed over silica gel (CH2Cl2 /methanol/triethylamine 9/1/0.1)

実験手順

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).

出典