Chlorodifluoromethane → Ethyl 1,1-diethoxyethyl(difluoromethyl)phosphinate

HRID 2050729노트

반응식

HRID 2050729 반응식
[H-].[Na+].[CH2:3]([O:5][C:6]([PH:11](=[O:15])[O:12][CH2:13][CH3:14])([O:8][CH2:9][CH3:10])[CH3:7])[CH3:4].Cl[CH:17]([F:19])[F:18]>O1CCCC1>[CH2:9]([O:8][C:6]([P:11]([CH:17]([F:19])[F:18])(=[O:15])[O:12][CH2:13][CH3:14])([O:5][CH2:3][CH3:4])[CH3:7])[CH3:10]

참가 물질

5

반응물 3

HCID 6372ChlorodifluoromethaneHCID 24758Sodium hydrideHCID 178476820HCID 178476820, 화합물

생성물 1

HCID 9992738Ethyl 1,1-diethoxyethyl(difluoromethyl)phosphinate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of 15.8 g of sodium hydride (dispersion in oil) in 500 ml of tetrahydrofuran are added dropwise 67 g (300 mMol) of ethyl 1,1-diethoxyethylphosphinate at such a rate so that the temperature, exceed 25° C. This mixture is stirred for one hour at room temperature, then cooled to -10° C. and 77.8 g (900 mMol) of chlorodifluoromethane are introduced. Stirring is continued for another 2 hours at room temperature, then 100 ml of ice-cold water are added. The mixture is extracted three times with dichloromethane and the combined extracts dried over magnesium sulphate. Removal of the solvent in vacuo gives ethyl 1,1-diethoxyethyl(difluoromethyl)phosphinate as a viscous oil, Rf=0.44 (CH2Cl2 /CH3COOH, 9+1).

후처리

  1. customexceed 25° C
  2. temperaturecooled to -10° C.
  3. stirringStirring
  4. waitis continued for another 2 hours at room temperature
  5. extractionThe mixture is extracted three times with dichloromethane
  6. dry with materialthe combined extracts dried over magnesium sulphate
  7. customRemoval of the solvent in vacuo

출처 및 근거

ORD 기록
ord-d535c63ca0d741e891fc371df0dee78c
출처 데이터셋
uspto-grants-1991_05
특허 번호
US05013863

반응 노트

불러오는 중…