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

HRID 971616

反応式

HRID 971616 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-ac09a966d7ec4b7584b24e5a8f44cc6d
出典データセット
uspto-grants-1979_07
特許番号
US04160794

関連ノート

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