Water → 3-(3-Nitro-phenyl)-acrylonitrile

HRID 1837515

반응식

HRID 1837515 반응식
[C:1]([CH2:3]P(=O)(OCC)OCC)#[N:2].[H-].[Na+].[N+:14]([C:17]1[CH:18]=[C:19]([CH:22]=[CH:23][CH:24]=1)[CH:20]=O)([O-:16])=[O:15].O>O1CCCC1>[N+:14]([C:17]1[CH:18]=[C:19]([CH:20]=[CH:3][C:1]#[N:2])[CH:22]=[CH:23][CH:24]=1)([O-:16])=[O:15]

참가 물질

6

반응물 4

HCID 962WaterHCID 74493-NitrobenzaldehydeHCID 24758Sodium hydrideHCID 75676Diethyl (cyanomethyl)phosphonate

생성물 1

HCID 556693-(3-Nitro-phenyl)-acrylonitrile

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

At 0° C., 75.5 g of diethyl cyanomethylphosphonate dissolved in tetrahydrofuran are poured into a suspension of sodium hydride in tetrahydrofuran. After 30 minutes' contact at ambient temperature, 56 g of 3-nitrobenzaldehyde dissolved in tetrahydrofuran are poured in. After 1 hour, hydrolysis is carried out with 300 ml of water and then the solvent is concentrated. Following extraction with dichloromethane, washing the organic phase with water, drying over magnesium sulphate and concentration, the precipitate is taken up in diethyl ether and filtered off.

후처리

  1. additionare poured in
  2. waitAfter 1 hour
  3. customhydrolysis
  4. concentrationthe solvent is concentrated
  5. extractionextraction with dichloromethane
  6. washwashing the organic phase with water
  7. dry with materialdrying over magnesium sulphate and concentration
  8. filtrationfiltered off

출처 및 근거

ORD 기록
ord-83ff63ba8c864af485b35e9f901d6e97
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06784183B2

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