Chloroform → Ethyl 3-oxobutyl(diethoxymethyl)phosphinate

HRID 5170

반응식

HRID 5170 반응식
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]

참가 물질

5

반응물 3

HCID 6212ChloroformHCID 6570Methyl vinyl ketoneHCID 178418659HCID 178418659, 화합물

생성물 1

HCID 14362820Ethyl 3-oxobutyl(diethoxymethyl)phosphinate

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-30eae213606d47d0a395349b420efeef
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05243062

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