Allyl Alcohol → Allyl P,P-diethylphosphonoacetate

HRID 52872

반응식

HRID 52872 반응식
[CH2:1]([O:3][P:4]([CH2:9][C:10]([OH:12])=[O:11])([O:6][CH2:7][CH3:8])=[O:5])[CH3:2].[CH2:13](O)[CH:14]=[CH2:15].Cl.C(N=C=NCCCNC)C>C(Cl)Cl.CN(C)C1C=CN=CC=1>[CH2:7]([O:6][P:4]([CH2:9][C:10]([O:12][CH2:15][CH:14]=[CH2:13])=[O:11])([O:3][CH2:1][CH3:2])=[O:5])[CH3:8]

참가 물질

6

반응물 3

HCID 7858Allyl AlcoholHCID 36704(Diethoxyphosphinyl)acetic acidHCID 9794023N-(3-methylaminopropyl)-N'-ethylcarbodiimide hydrochloride

생성물 1

HCID 4583084Allyl P,P-diethylphosphonoacetate수율 82.2%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  1. additionwere added
  2. temperatureunder cooling with ice
  3. stirringThe mixture was stirred at room temperature overnight
  4. customThe reaction solution was evaporated under reduced pressure
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. washsequentially washed with 1N hydrochloric acid, water
  7. dry with materiala saturated sodium hydrogencarbonate aqueous solution and a saturated sodium chloride aqueous solution, and dried over anhydrous magnesium sulfate
  8. customThe drying agent was separated by filtration
  9. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-d728077f295740f79612ef0dd40891fd
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616803

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