2-Propenal, 3-[4-(1,1-dimethylethyl)phenyl]-2-methyl- → Lilial

HRID 1903318

반응식

HRID 1903318 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([CH:11]=[C:12]([CH:14]=[O:15])[CH3:13])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[H][H]>O.[Pd]>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([CH2:11][CH:12]([CH3:13])[CH:14]=[O:15])=[CH:9][CH:10]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 2

HCID 1146592-Propenal, 3-[4-(1,1-dimethylethyl)phenyl]-2-methyl-HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 228987Lilial수율 88.9%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

반응 조건

온도
110 °C

실험 절차

1420 g of 1-(p-tert.butylphenyl)-2-formyl-1-propene, prepared as described in paragraph (e), are mixed together with 6 g of 5% palladium/carbon and 6.8 g of soda in 20 ml of water at 70°-75° C. in a stirring autoclave. The autoclave is charged with hydrogen (8 atmospheres) and heated to 110° C. About 230 liters of hydrogen are absorbed after 12 hours. The crude 3-(p-tert.butyl-phenyl)-2-methyl-propionaldehyde is treated with ether, washed neutral with water and dried over sodium sulphate. After removing the ether, the product is fractionally distilled in vacuo. After separating a first running and a last running, there are obtained 1275 g of 3-(p-tert.butylphenyl)-2-methyl-propionaldehyde in 95% purity (about 88% of theory). Boiling point: 150°-152° C./15 mmHg; nD20 =1.5050.

후처리

  1. customAbout 230 liters of hydrogen are absorbed after 12 hours
  2. additionThe crude 3-(p-tert.butyl-phenyl)-2-methyl-propionaldehyde is treated with ether
  3. washwashed neutral with water
  4. dry with materialdried over sodium sulphate
  5. customAfter removing the ether
  6. distillationthe product is fractionally distilled in vacuo
  7. customAfter separating a first running

출처 및 근거

ORD 기록
ord-41740ed71faf4bc78ef173ba5d954b0f
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04435585

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