Methyl Acrylate → 1,1,3-Trichloro-3-carbomethoxypropane-1-phosphonic dichloride

HRID 1438901

반응식

HRID 1438901 반응식
[Cl:1][C:2]([Cl:8])(Cl)[P:3]([Cl:6])([Cl:5])=[O:4].[CH3:9][O:10][C:11](=[O:14])[CH:12]=[CH2:13].[Cl-:15].C([NH+](CC)CC)C>C(#N)C>[Cl:1][C:2]([Cl:8])([P:3]([Cl:6])([Cl:5])=[O:4])[CH2:13][CH:12]([Cl:15])[C:11]([O:10][CH3:9])=[O:14]

참가 물질

5

반응물 3

HCID 7294Methyl AcrylateHCID 277422(Trichloromethyl)phosphonic dichlorideHCID 12698378Triethylazanium chloride

생성물 1

HCID 213996741,1,3-Trichloro-3-carbomethoxypropane-1-phosphonic dichloride

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To 11.8 g (0.05 mole) distilled trichloromethane phosphonic dichloride and 8.6 g (0.1 mole) methylacrylate was added a solution of 134 mg (1 mmole) anhydrous cupric chloride and 206 mg (1.5 mmole) triethylammonium chloride in 5 ml acetonitrile. The homogeneous solution was heated in the absence of air in a sealed ampoule at 125° for 15 hours. After cooling, the contents of the ampoule was subjected to distillation. 12.9 g 1:1 adduct, 1,1,3-trichloro-3-carbomethoxypropane-1-phosphonic dichloride was obtained, bp/0.04: 83°. Cl-(by half-hydrolysis): 11.23%. Calc. for C5H6Cl5O2P: 11.01%. In the absence of triethylammonium chloride, 3.7 g adduct was obtained.

후처리

  1. temperatureThe homogeneous solution was heated in the absence of air in a sealed ampoule at 125° for 15 hours
  2. temperatureAfter cooling
  3. distillationthe contents of the ampoule was subjected to distillation

출처 및 근거

ORD 기록
ord-d2dc2003ec234f27acb0742daf0cba66
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04057578

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