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Acetone → HCID 13656344, Verbindung

HRID 979719
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 979719
CC(C)=O.[Cl:5][C:6]1[CH:7]=[C:8]([N:12]([CH3:16])[C:13](Cl)=[O:14])[CH:9]=[CH:10][CH:11]=1.[C:17]([C:21]1[CH:22]=[C:23]([OH:28])[CH:24]=[CH:25][C:26]=1[Cl:27])([CH3:20])([CH3:19])[CH3:18].C(=O)([O-])[O-].[K+].[K+]>O>[Cl:5][C:6]1[CH:7]=[C:8]([N:12]([CH3:16])[C:13](=[O:14])[O:28][C:23]2[CH:24]=[CH:25][C:26]([Cl:27])=[C:21]([C:17]([CH3:20])([CH3:18])[CH3:19])[CH:22]=2)[CH:9]=[CH:10][CH:11]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 180AcetoneHCID 11430Potassium CarbonateHCID 109102303-Tert-butyl-4-chlorophenolHCID 13882387HCID 13882387, Verbindung

Produkt 1

HCID 13656344HCID 13656344, VerbindungAusbeute 91,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962
Water
Lösungsmittel

Versuchsvorschrift

To 30 ml of acetone were added 2.04 g of N-(3-chlorophenyl)-N-methylcarbamoyl chloride, 1.84 g of 3-tert-butyl-4-chlorophenol and 1.6 g of anhydrous potassium carbonate, and the mixture was refluxed with heating for 48 hours. The reaction mixture was cooled down to room temperature and thereafter was poured into cold water. The product was extracted with benzene. The benzene solution was washed with water and a saturated aqueous solution of sodium chloride in this order, and was dried over anhydrous magnesium sulfate. Thereafter, benzene was distilled off. The residue was purified through a column chromatography (employing silica gel as carrier and benzen as developing solvent), and further recrystallized from hexane to give 3.2 g of 3-tert-butyl-4-chlorophenyl N-(3-chlorophenyl)-N-methylcarbamate, having melting point of 65°-67° C.

Aufarbeitung

  1. temperaturethe mixture was refluxed
  2. temperaturewith heating for 48 hours
  3. extractionThe product was extracted with benzene
  4. washThe benzene solution was washed with water
  5. dry with materiala saturated aqueous solution of sodium chloride in this order, and was dried over anhydrous magnesium sulfate
  6. distillationThereafter, benzene was distilled off
  7. customThe residue was purified through a column chromatography (employing silica gel as carrier and benzen as developing solvent)
  8. customfurther recrystallized from hexane

Quellen und Nachweise

ORD-Eintrag
ord-c62ccf94b4cd4514b1669a2aa44d13c7
Quelldatensatz
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04668831

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