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

HRID 729156ノート

反応式

HRID 729156 の反応式
[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]

参加物

5

反応物 3

HCID 6372ChlorodifluoromethaneHCID 24758Sodium hydrideHCID 178476820HCID 178476820、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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 does not 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).

後処理

  1. customdoes not exceed 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

出典と根拠

ORDレコード
ord-02fe391efa80496fa3c2b41223b9a2b8
出典データセット
uspto-grants-1991_09
特許番号
US05051524

反応ノート

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