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

HRID 67269ノート

反応式

HRID 67269 の反応式
[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]

参加物

4

反応物 2

HCID 8472Trimethyl phosphite2 回HCID 110450293-Iodo-2-(iodomethyl)prop-1-ene

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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;

後処理

  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

出典と根拠

ORDレコード
ord-68c07a8e9c60486885b3dfcde221822a
出典データセット
uspto-grants-1982_08
特許番号
US04346023

反応ノート

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