Triethylamine → 1-(4-Chlorobenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine

HRID 67076Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 67076
Cl.[NH:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][N:4]([CH:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[C:3]1=[O:18].Br[CH2:20][C:21]([C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=1)=[O:22].C(N(CC)CC)C>CO>[Cl:29][C:26]1[CH:27]=[CH:28][C:23]([C:21]([CH2:20][N:15]2[CH2:14][CH2:13][CH:12]([N:4]3[CH2:5][C:6]4[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=4)[NH:2][C:3]3=[O:18])[CH2:17][CH2:16]2)=[O:22])=[CH:24][CH:25]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 68303p-Chlorophenacyl bromideHCID 183213553-(Piperidin-4-yl)-3,4-dihydroquinazolin-2(1H)-one hydrochloride

Produkt 1

HCID 127979931-(4-Chlorobenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidineAusbeute 56 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

In this example, 4.0 g of 4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine mono-hydrochloride, 3.5 g of α-bromo-p-chloroacetophenone, 4.2 ml of triethylamine and 60 ml of methanol are mixed and stirred at room temperature overnight. The white crystals deposited are separated by filtration, successively washed with methanol and water and dried to obtain 5.17 g of a crude product. The crude product is recrystallized from a mixed solvent of chloroform and ethanol to obtain 3.21 g of the desired product.

Aufarbeitung

  1. customThe white crystals deposited are separated by filtration
  2. washsuccessively washed with methanol and water
  3. customdried
  4. customto obtain 5.17 g of a crude product
  5. customThe crude product is recrystallized from a mixed solvent of chloroform and ethanol

Quellen und Nachweise

ORD-Eintrag
ord-609aaef785044093b5b2a20a3ab02518
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04344948

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