Реакция #81150

Уравнение реакции

diethylphosphonoacetic acid

allyl alcohol

1-ethyl-3-(3-methylaminopropyl)carbodiimide hydrochloride

→

allyl diethylphosphonoacetate

Выход 82.2%

Растворители

methylene chloride

Условия реакции

Обработка

1. 1
   workup.ADDITIONwere added
2. 2
   Температураunder cooling with ice
3. 3
   workup.STIRRINGThe mixture was stirred at room temperature overnight
4. 4
   ДругоеThe reaction solution was evaporated under reduced pressure
5. 5
   workup.DISSOLUTIONThe residue was dissolved in ethyl acetate
6. 6
   Промывкаsequentially washed with 1N hydrochloric acid, water
7. 7
   Сушкаa saturated sodium hydrogencarbonate aqueous solution and a saturated sodium chloride aqueous solution, and dried over anhydrous magnesium sulfate
8. 8
   ДругоеThe drying agent was separated by filtration
9. 9
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

Методика

29.2 g of the diethylphosphonoacetic acid thus obtained was dissolved in 350 me of methylene chloride, and 17.8 g of allyl alcohol, 1.92 g of 4-dimethylaminopyridine and 29.0 g of 1-ethyl-3-(3-methylaminopropyl)carbodiimide hydrochloride were added thereto with stirring under cooling with ice. The mixture was stirred at room temperature overnight. The reaction solution was evaporated under reduced pressure. The residue was dissolved in ethyl acetate, then sequentially washed with 1N hydrochloric acid, water, a saturated sodium hydrogencarbonate aqueous solution and a saturated sodium chloride aqueous solution, and dried over anhydrous magnesium sulfate. The drying agent was separated by filtration, and then the solvent was distilled off under reduced pressure to obtain 28.9 g of allyl diethylphosphonoacetate.

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