Oxygen → 1-Methyl-1-oxophospholanyl methyl phosphinic acid methyl ester

HRID 972305

反応式

HRID 972305 の反応式
[CH3:1][P:2]1(=[O:7])[CH2:6][CH2:5][CH:4]=[CH:3]1.O=O.[CH3:10][O:11][P:12]([CH3:14])[OH:13]>>[CH3:10][O:11][P:12]([CH:3]1[CH2:4][CH2:5][CH2:6][P:2]1([CH3:1])=[O:7])([CH3:14])=[O:13]

参加物

4

反応物 3

HCID 977OxygenHCID 701042,3-Dihydro-1-methyl-1H-phosphole 1-oxideHCID 54069057Methane phosphonous acid methyl ester

生成物 1

HCID 538809981-Methyl-1-oxophospholanyl methyl phosphinic acid methyl ester収率 277.5%

実験手順

A total of 116 g of 1-methyl-1-oxophospholine and 6 g of tert.-butyl peroctoate in 30 g of methane phosphonous acid methyl ester are simultaneously added dropwise with stirring at 120° C to 282 g of oxygen-free methane phosphonous acid methyl ester. The reaction time is 90 minutes. Excess methane phosphonous acid methyl ester and a little 1-methyl oxophospholine are distilled off. For purification, the residue of 205 g of 1-methyl-1-oxophospholanyl methyl phosphinic acid methyl ester is distilled in vacuo (b.p. 210° -220° C) and gives 186 g of a pure product which hardens very slowly into star-shaped crystals which become liquid again at a temperature above 70° C.

後処理

  1. distillationExcess methane phosphonous acid methyl ester and a little 1-methyl oxophospholine are distilled off
  2. customFor purification
  3. distillationthe residue of 205 g of 1-methyl-1-oxophospholanyl methyl phosphinic acid methyl ester is distilled in vacuo (b.p. 210° -220° C)

出典と根拠

ORDレコード
ord-90f8c4e4f56e479ba54f350c648879f2
出典データセット
uspto-grants-1977_10
特許番号
US04052484

関連ノート

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