Triethylamine → 4-Methyl-4-(3,5-di-tert-butyl-4-hydroxyphenylthio)-2-pentanone

HRID 65167

Reaktionsgleichung

Reaktionsgleichung von HRID 65167
[O:1]=[C:2]([CH:4]=[C:5]([CH3:7])[CH3:6])[CH3:3].[C:8]([C:12]1[CH:17]=[C:16]([SH:18])[CH:15]=[C:14]([C:19]([CH3:22])([CH3:21])[CH3:20])[C:13]=1[OH:23])([CH3:11])([CH3:10])[CH3:9].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH3:6][C:5]([S:18][C:16]1[CH:15]=[C:14]([C:19]([CH3:20])([CH3:21])[CH3:22])[C:13]([OH:23])=[C:12]([C:8]([CH3:11])([CH3:10])[CH3:9])[CH:17]=1)([CH3:7])[CH2:4][C:2](=[O:1])[CH3:3]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 8858Mesityl oxideHCID 703702,6-Di-tert-butyl-4-mercaptophenol

Produkt 1

HCID 136435724-Methyl-4-(3,5-di-tert-butyl-4-hydroxyphenylthio)-2-pentanone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

8.48 Grams of mesityl oxide (0.084 moles) is added dropwise to a solution of 21.0 grams of 2,6 di-tert-butyl-4-mercaptophenol (0.088 moles) and one gram of triethylamine in 30 ml of toluene. The mixture is heated at 50°-55° C. for six hours. The solvent is then stripped off under vacuum and the residue retained at 60°-65° C. and 0.20 mm. Hg. for two hours. The residue is dissolved in toluene and purified by flash chromatography using silica gel. The product is isolated from solution by distilling off the volatiles under vacuum to a final pressure of 0.10 mm. Hg for five hours.

Aufarbeitung

  1. temperatureThe mixture is heated at 50°-55° C. for six hours
  2. customretained at 60°-65° C.
  3. custompurified by flash chromatography
  4. customThe product is isolated from solution
  5. distillationby distilling off the volatiles under vacuum to a final pressure of 0.10 mm. Hg for five hours

Quellen und Nachweise

ORD-Eintrag
ord-d4de8aeca9ca45eda5bfc5d0c2ea9d50
Quelldatensatz
uspto-grants-1986_09
Patentnummer
US04612341

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