1,4'-Bipiperidine → 3,5-Dimethyl-2-[4-[4-[2-(4-piperidinopiperidino)-ethoxy]benzoyl]benzylthio]-4(3H)-quinazolinone dihydrochloride

HRID 1291379Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1291379
[Cl:1][CH2:2][CH2:3][O:4][C:5]1[CH:33]=[CH:32][C:8]([C:9]([C:11]2[CH:31]=[CH:30][C:14]([CH2:15][S:16][C:17]3[N:26]([CH3:27])[C:25](=[O:28])[C:24]4[C:19](=[CH:20][CH:21]=[CH:22][C:23]=4[CH3:29])[N:18]=3)=[CH:13][CH:12]=2)=[O:10])=[CH:7][CH:6]=1.[N:34]1([CH:40]2[CH2:45][CH2:44][NH:43][CH2:42][CH2:41]2)[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1>CN(C=O)C>[ClH:1].[ClH:1].[CH3:27][N:26]1[C:25](=[O:28])[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][C:23]=2[CH3:29])[N:18]=[C:17]1[S:16][CH2:15][C:14]1[CH:30]=[CH:31][C:11]([C:9](=[O:10])[C:8]2[CH:32]=[CH:33][C:5]([O:4][CH2:3][CH2:2][N:43]3[CH2:44][CH2:45][CH:40]([N:34]4[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]4)[CH2:41][CH2:42]3)=[CH:6][CH:7]=2)=[CH:12][CH:13]=1

Komponenten

4

Edukt 2

HCID 786071,4'-BipiperidineHCID 189188132-[4-[4-(2-Chloroethoxy)benzoyl]benzylthio]-3,5-dimethyl-4(3H)-quinazolinone

Produkt 1

HCID 189192323,5-Dimethyl-2-[4-[4-[2-(4-piperidinopiperidino)-ethoxy]benzoyl]benzylthio]-4(3H)-quinazolinone dihydrochlorideAusbeute 137,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 2-[4-[4-(2-chloroethoxy)benzoyl]benzylthio]-3,5-dimethyl-4(3H)-quinazolinone (375 mg) and 4-piperidinopiperidine (434 mg) in DMF (5 ml) was stirred at 100° C. for 7 hours. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate, washed with water, dried, and concentrated. Then, hydrogen chloride/ethyl acetate was added and the precipitated hydrochloride was recovered by filtration and dried to provide the title compound as colorless solid (368 mg).

Aufarbeitung

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated
  6. additionThen, hydrogen chloride/ethyl acetate was added
  7. filtrationthe precipitated hydrochloride was recovered by filtration
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-449dd8d14ef349439cf551a2e47c5cf0
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05753664

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