Hydrochloric Acid → 1-Oxo-2-(2-diethylphosphonoethyl)-2-methoxy-1,2-diphenylethane

HRID 971616

반응식

HRID 971616 반응식
[CH3:1][O:2][CH:3]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:4](=[O:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[OH-].[Na+].[CH:20]([P:22](=[O:29])([O:26][CH2:27][CH3:28])[O:23][CH2:24][CH3:25])=[CH2:21].Cl>CS(C)=O>[O:11]=[C:4]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[C:3]([CH2:21][CH2:20][P:22]([O:26][CH2:27][CH3:28])([O:23][CH2:24][CH3:25])=[O:29])([O:2][CH3:1])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 69629Diethyl vinylphosphonateHCID 98097Methyl Benzoin

생성물 1

HCID 545302481-Oxo-2-(2-diethylphosphonoethyl)-2-methoxy-1,2-diphenylethane

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

16.4 g. (0.1 mole) of benzoin methyl ether are dissolved in 100 ml of dimethyl sulphoxide. While passing in nitrogen, 3 ml of 4 normal sodium hydroxide solution are added dropwise. Then 18 g (0.11 mole) of diethyl vinylphosphonate are added dropwise in the course of 10 minutes. The reaction mixture is stirred for 16 hours at room temperature under nitrogen and subsequently neutralised with 2 normal hydrochloric acid. After the reaction mixture has been completely concentrated under reduced pressure, the oily residue is taken up in toluene, washed twice with water and again completely concentrated by rotary evaporation to yield 1-oxo-2-(2-diethylphosphonoethyl)-2-methoxy-1,2-diphenylethane as a slightly viscous yellowish oil which crystallises on standing; m.p. 60°-62° C. (initiator 1).

후처리

  1. concentrationAfter the reaction mixture has been completely concentrated under reduced pressure
  2. washwashed twice with water
  3. concentrationagain completely concentrated by rotary evaporation

출처 및 근거

ORD 기록
ord-ac09a966d7ec4b7584b24e5a8f44cc6d
출처 데이터셋
uspto-grants-1979_07
특허 번호
US04160794

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