Toluene → HCID 12939724, Verbindung

HRID 1577466Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1577466
C1(C)C=CC=CC=1.[CH3:8][C:9]([NH2:17])([CH3:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[Cl:18][CH:19]([C:23]([CH3:26])([CH3:25])[CH3:24])[C:20](Cl)=[O:21]>N1C=CC=CC=1>[CH3:8][C:9]([NH:17][C:20](=[O:21])[CH:19]([C:23]([CH3:26])([CH3:25])[CH3:24])[Cl:18])([CH3:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

Komponenten

5

Edukt 3

HCID 1140TolueneHCID 68509CumylamineHCID 12239723Butanoyl chloride, 2-chloro-3,3-dimethyl-

Produkt 1

HCID 12939724HCID 12939724, VerbindungAusbeute 88,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

Into a 200 ml four-necked flask, there were charged toluene (100 ml), α,α-dimethylbenzylamine (9 g) and pyridine (5.8 g), and α-chloro-tert-butylacetyl chloride (11.3 g) was dropwise added thereto while stirring at room temperature. Stirring was continued for 3 hours. The reaction mixture was washed with water to remove pyridine hydrochloride. After the toluene layer was dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The obtained residue was recrystallized from ethanol to give 15.8 g of N-(α,α-dimethylbenzyl)-α-chloro-tert-butylacetamide. M.P., 159°-160° C.

Aufarbeitung

  1. additionwas dropwise added
  2. stirringStirring
  3. washThe reaction mixture was washed with water
  4. customto remove pyridine hydrochloride
  5. dry with materialAfter the toluene layer was dried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe obtained residue was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-8608a004a37241d7b420be51d9ac667e
Quelldatensatz
uspto-grants-1981_09
Patentnummer
US04288244

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