Trimethyl phosphite → 1,3-Bis(dimethylphosphono)-2-methylene-propane

HRID 1155587노트

반응식

HRID 1155587 반응식
[P:1]([O:6]C)([O:4][CH3:5])[O:2][CH3:3].I[CH2:9][C:10]([CH2:12]I)=[CH2:11]>C1C=CC=CC=1>[CH3:3][O:2][P:1]([CH2:9][C:10](=[CH2:11])[CH2:12][P:1]([O:2][CH3:3])([O:4][CH3:5])=[O:6])([O:4][CH3:5])=[O:6]

참가 물질

4

반응물 2

HCID 8472Trimethyl phosphite2회HCID 110450293-Iodo-2-(iodomethyl)prop-1-ene

생성물 1

HCID 205268441,3-Bis(dimethylphosphono)-2-methylene-propane수율 92%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

400 ml of trimethyl phosphite was placed into a 2-1 flask equipped with an addition funnel, a gas inlet tube, and a Vigreux column with distilling head. The phosphite was heated at reflux, then a solution of 131 g (0.425 Mole) of 2-iodomethyl-3-iodopropene [see J. Amer. Chem. Soc., 89, 4688 (1967)] in 200 ml of benzene was added dropwise over a period of 2 h, followed by an additional 100 ml of trimethyl phosphite within 30 min. The reaction was run under nitrogen, and approx. 150 ml of distillate was allowed to collect. Distillation of the reaction mixture afforded 106 g (92%) of the title compound, b.p. 125°-7°/0.08 Torr;

후처리

  1. customequipped with an addition funnel, a gas inlet tube
  2. distillationa Vigreux column with distilling head
  3. temperatureThe phosphite was heated
  4. temperatureat reflux
  5. customto collect
  6. distillationDistillation of the reaction mixture

출처 및 근거

ORD 기록
ord-508ef7df59f04d7589d21119dff6ea89
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04302607

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