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

HRID 1837515

反応式

HRID 1837515 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-83ff63ba8c864af485b35e9f901d6e97
出典データセット
uspto-grants-2004_08
特許番号
US06784183B2

関連ノート

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