Chloroform → Ethyl 3-oxobutyl(diethoxymethyl)phosphinate

HRID 5170

反応式

HRID 5170 の反応式
C[Si]([PH:5]([CH:10]([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])([O-:9])[O:6][CH2:7][CH3:8])(C)C.[CH:17]([C:19]([CH3:21])=[O:20])=[CH2:18].C(Cl)(Cl)Cl>O>[O:20]=[C:19]([CH3:21])[CH2:17][CH2:18][P:5]([CH:10]([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])(=[O:9])[O:6][CH2:7][CH3:8]

参加物

5

反応物 3

HCID 6212ChloroformHCID 6570Methyl vinyl ketoneHCID 178418659HCID 178418659、化合物

生成物 1

HCID 14362820Ethyl 3-oxobutyl(diethoxymethyl)phosphinate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

15.0 g of ethyl trimethylsilyl(diethoxymethyl)phosphonite are added dropwise to a stirred solution of 3.9 g of methyl vinyl ketone under an atmosphere of nitrogen at room temperature. The mixture is then heated to 50° C. for a period of 1 hour. The mixture is then allowed to cool to room temperature, 25 ml of chloroform is then added followed by 10 ml water and this mixture is vigorously stirred for a period of 0.5 h. The organic layer is then separated, dried over magnesium sulphate and concentrated under reduced pressure and the crude product distilled under reduced pressure to give ethyl 3-oxobutyl(diethoxymethyl)phosphinate, b.p. 130°-135° C./0.02 mbar, 31P=+45.3 ppm (CDCl3).

後処理

  1. temperatureto cool to room temperature
  2. customThe organic layer is then separated
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated under reduced pressure
  5. distillationthe crude product distilled under reduced pressure

出典と根拠

ORDレコード
ord-30eae213606d47d0a395349b420efeef
出典データセット
uspto-grants-1993_09
特許番号
US05243062

関連ノート

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