Acetic Acid → 2-Pentenal, 2-methyl-4-phenyl-

HRID 246985

反応式

HRID 246985 の反応式
[CH:1](=[O:4])[CH2:2][CH3:3].[C:5]1([CH:11]([CH3:14])[CH:12]=O)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[OH-].[Na+].C(O)(=O)C>CO>[CH3:3][C:2](=[CH:12][CH:11]([CH3:14])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[CH:1]=[O:4]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 527PropanalHCID 71462-PhenylpropanalHCID 14798Sodium Hydroxide

生成物 1

HCID 570411602-Pentenal, 2-methyl-4-phenyl-収率 34.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

192 g of propionaldehyde are added dropwise to a solution of 402 g of 2-phenylpropan-1-al and 12 g of sodium hydroxide in 1 l of methanol in the course of 6 hours. Stirring is continued for one hour, after which the mixture is neutralized with glacial acetic acid (pH=6), stirred overnight and evaporated down, the residue is taken up with CH2Cl2 /H2O, and the solution is extracted with CH2Cl2. The organic phase is washed with water, dried over Na2SO4, evaporated down again and distilled to give 178 g of 2,4-dimethyl-4-phenylbut-2-en-1-al of boiling point 108°-120° C./0.5 mbar.

後処理

  1. stirringstirred overnight
  2. customevaporated down
  3. extractionthe solution is extracted with CH2Cl2
  4. washThe organic phase is washed with water
  5. dry with materialdried over Na2SO4
  6. customevaporated down again
  7. distillationdistilled

出典と根拠

ORDレコード
ord-0f72f826f034420aaea23dd9c9ace2bb
出典データセット
uspto-grants-1987_11
特許番号
US04705553

関連ノート

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