Pyridine → Di-(2-ethylthioethyl)2-chloroethanephosphonate

HRID 1449302

반응식

HRID 1449302 반응식
[Cl:1][CH2:2][CH2:3][P:4](Cl)(Cl)=[O:5].[CH2:8]([S:10][CH2:11][CH2:12][OH:13])[CH3:9].N1[CH:19]=[CH:18]C=CC=1>CCOCC>[CH2:8]([S:10][CH2:11][CH2:12][O:13][P:4]([CH2:3][CH2:2][Cl:1])(=[O:5])[O:13][CH2:12][CH2:11][S:10][CH2:18][CH3:19])[CH3:9]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 80752-(Ethylthio)ethanolHCID 69645(2-Chloroethyl)phosphonic dichloride

생성물 1

HCID 85916432Di-(2-ethylthioethyl)2-chloroethanephosphonate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a solution of 18.1 g (0.1 mol) of 2-chloroethane phosphonic acid dichloride in 150 ml of absolute ether is added dropwise with stirring a solution of 21.2 g (0.2 mol) of hydroxyethyl ethyl sulphide and 15.8 g of absolute pyridine in 100 ml of absolute ether at room temperature, during which the temperature increases to 35° and crystallisation occurs. Stirring is continued for a further 14 hours at 25° after which the crystals are removed by filtration and the ethereal filtrate is washed to neutrality with 5% hydrogen carbonate solution and water. It is dried and evaporated and further dried by rotation under high vacuum for 2 hours. A yellow oil is obtained having the following characterisation data:

후처리

  1. temperatureduring which the temperature increases to 35°
  2. customcrystallisation
  3. customafter which the crystals are removed by filtration
  4. washthe ethereal filtrate is washed
  5. customIt is dried
  6. customevaporated
  7. customfurther dried by rotation under high vacuum for 2 hours
  8. customA yellow oil is obtained

출처 및 근거

ORD 기록
ord-13e9384b72ff4f8c82a8c6f56f8594b2
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04190430

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