Реакция #5012

ord-3b1908a01a5143ef967011e4244289b7

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05242908uspto-grants-1993_09