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

HRID 1030677

Reaktionsgleichung

Reaktionsgleichung von HRID 1030677
[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]

Komponenten

5

Edukt 3

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

Produkt 1

HCID 11687311Ethanone, 1-[2,4,6-trihydroxy-3-(3-methyl-2-butenyl)phenyl]-Ausbeute 34 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

In tetrahydrofuran were dissolved and suspended 66.5 g of 2',4',6'-trihydroxyacetophenone and 173.0 g of potassium carbonate, and 56.0 ml of 1-chloro-3-methyl-2-butene was dropped into the solution. The mixture was stirred at room temperature for 2 hours and extracted with dimethyl ether, and the organic layer was washed with a 5% solution of potassium carbonate and then with water. The organic layer was shaken with a saturated solution of sodium chloride, dried with anhydrous sodium sulfate and concentrated under a reduced pressure. Recrystallization from benzene gave 31.8 g (yield=34.0%) of 2',4',6'-trihydroxy-3'-(3-methyl-2-butenyl)acetophenone.

Aufarbeitung

  1. additionwas dropped into the solution
  2. extractionextracted with dimethyl ether
  3. washthe organic layer was washed with a 5% solution of potassium carbonate
  4. stirringThe organic layer was shaken with a saturated solution of sodium chloride
  5. dry with materialdried with anhydrous sodium sulfate
  6. concentrationconcentrated under a reduced pressure
  7. customRecrystallization from benzene

Quellen und Nachweise

ORD-Eintrag
ord-1a18efb07f9a4a748d27e8ba7dc9503e
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05106871

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