Acetic Acid → 2-Cyanoethyl(n-butyl)phosphinic acid ethyl ester

HRID 483998노트

반응식

HRID 483998 반응식
[CH2:1]([O:3][P:4]([CH2:7][CH2:8][CH2:9][CH3:10])(=[O:6])O)[CH3:2].[C:11](#[N:14])[CH:12]=[CH2:13].[Na].C(O)(=O)C>C(O)C>[CH2:1]([O:3][P:4]([CH2:13][CH2:12][C:11]#[N:14])([CH2:7][CH2:8][CH2:9][CH3:10])=[O:6])[CH3:2]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 7855AcrylonitrileHCID 5272049Butyl(ethoxy)phosphinic acidHCID 5360545Sodium

생성물 1

HCID 104428632-Cyanoethyl(n-butyl)phosphinic acid ethyl ester

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

15.0 g of n-butylphosphonic acid ethyl ester and 5.3 g of acrylonitrile are dissolved under argon in 25 ml of ethanol. The solution is cooled to 10°, and a solution of 1.15 g of sodium in 50 ml of ethanol is added dropwise, whereupon an exothermic reaction takes place. The mixture is then heated under reflux for one hour and cooled to room temperature, and 3.3 g of glacial acetic acid are added. The solvent is removed and the residue is taken up in dichloromethane. The resulting solution is washed with water, dried over sodium sulfate and concentrated by evaporation. The oil that remains is distilled, yielding 2-cyanoethyl(n-butyl)phosphinic acid ethyl ester having a boiling point of 120° (10-1 bar).

후처리

  1. temperatureThe solution is cooled to 10°
  2. temperatureThe mixture is then heated
  3. temperatureunder reflux for one hour
  4. customThe solvent is removed
  5. washThe resulting solution is washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated by evaporation
  8. distillationThe oil that remains is distilled

출처 및 근거

ORD 기록
ord-14eef7d179e24bb3b6c93e2ce56336a9
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05229379

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