Methyl Ethyl Ketone → HCID 23333251, Verbindung

HRID 224471

Reaktionsgleichung

Reaktionsgleichung von HRID 224471
[CH3:1][C:2]1[CH:8]=[C:7]([OH:9])[C:6]([C:10](=[O:26])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])=[CH:5][C:3]=1[OH:4].C(=O)([O-])[O-].[K+].[K+].[CH2:33]([C:35](C)=O)[CH3:34].C(Br)C=C>O>[CH2:35]([O:4][C:3]1[CH:5]=[C:6]([C:10](=[O:26])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[C:7]([OH:9])=[CH:8][C:2]=1[CH3:1])[CH:33]=[CH2:34]

Komponenten

6

Edukt 4

HCID 6569Methyl Ethyl KetoneHCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 147165312-Methyl-5-hexadecanoylhydroquinone

Produkt 1

HCID 23333251HCID 23333251, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Under nitrogen atmosphere a mixture of 17.5 g of the keto-compound of step 1, 10.2 g of potassium carbonate and 200 ml of methyl ethyl ketone was refluxed with stirring together with 6.9 g of allyl bromide for 1 hour. After a total refluxing time of 9 h the reaction mixture was mixed with 100 ml of water. The methyl ethyl ketone layer is separated, shaken twice with a 20% by weight sodium chloride solution and dried with sodium sulphate. The residue left after evaporation of the solvent was stirred with methanol, whereupon the precipitate formed was filtered with suction and recrystallized from methanol.

Aufarbeitung

  1. temperaturewas refluxed
  2. customThe methyl ethyl ketone layer is separated
  3. dry with materialdried with sodium sulphate
  4. waitThe residue left
  5. customafter evaporation of the solvent
  6. stirringwas stirred with methanol, whereupon the precipitate
  7. customformed
  8. filtrationwas filtered with suction
  9. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-2d82cbf723b74eba9546114ca420b46a
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04232107

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