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

HRID 246985

반응식

HRID 246985 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0f72f826f034420aaea23dd9c9ace2bb
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705553

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