1-Chloro-3-methyl-2-butene → Ethanone, 1-[2,4,6-trihydroxy-3-(3-methyl-2-butenyl)phenyl]-

HRID 1030680

반응식

HRID 1030680 반응식
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[C:4]([OH:9])[C:3]=1[C:10](=[O:12])[CH3:11].C(=O)([O-])[O-].[K+].[K+].Cl[CH2:20][CH:21]=[C:22]([CH3:24])[CH3:23]>O1CCCC1>[OH:1][C:2]1[C:7]([CH2:20][CH:21]=[C:22]([CH3:24])[CH3:23])=[C:6]([OH:8])[CH:5]=[C:4]([OH:9])[C:3]=1[C:10](=[O:12])[CH3:11]

참가 물질

5

반응물 3

HCID 104291-Chloro-3-methyl-2-buteneHCID 11430Potassium CarbonateHCID 680732',4',6'-Trihydroxyacetophenone

생성물 1

HCID 11687311Ethanone, 1-[2,4,6-trihydroxy-3-(3-methyl-2-butenyl)phenyl]-수율 55%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In 250 ml of anhydrous tetrahydrofuran was dissolved 50.0 g of 2',4',6'-trihydroxyacetophenone, and 123.1 g of anhydrous potassium carbonate was added to the solution and the mixture was stirred at room temperature for 30 minutes. Then, 37.2 g of 1-chloro3-methyl-2-butene was added dropwise to the mixture over a period of 20 minutes and reaction was carried out at room temperature for 24 hours. After the reaction, the reaction mixture was extracted with 2 l of ethyl acetate and the solvent was removed from the ethyl acetate layer by distillation, and the residue was recrystallized from a benzene/petroleum ether mixed solvent to obtain 38.6 g (yield=55.0%) of 2',4',6'-trihydroxy-3'-(3-methyl-2-butenyl)acetophenone in the form of a yellow prism.

후처리

  1. additionwas added to the solution
  2. customreaction
  3. waitwas carried out at room temperature for 24 hours
  4. customAfter the reaction
  5. extractionthe reaction mixture was extracted with 2 l of ethyl acetate
  6. customthe solvent was removed from the ethyl acetate layer by distillation
  7. customthe residue was recrystallized from a benzene/petroleum ether mixed solvent

출처 및 근거

ORD 기록
ord-74e2a1ebf3ec4cde92c5887a9a38f149
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05106871

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