Potassium Carbonate → 3,5-Dimethyl-2-[4-[4-(2-piperidinoethoxy)benzoyl]-benzylthio]thieno[2,3-d]pyrimidin-4(3H)-one hydrochloride

HRID 1291350Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1291350
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[C:9]([CH3:12])=[CH:10][S:11][C:5]=2[N:4]=[C:3]1[S:13][CH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21](=[O:29])[C:22]2[CH:27]=[CH:26][C:25]([OH:28])=[CH:24][CH:23]=2)=[CH:17][CH:16]=1.Cl.[Cl:31][CH2:32][CH2:33][N:34]1[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[ClH:31].[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[C:9]([CH3:12])=[CH:10][S:11][C:5]=2[N:4]=[C:3]1[S:13][CH2:14][C:15]1[CH:16]=[CH:17][C:18]([C:21](=[O:29])[C:22]2[CH:23]=[CH:24][C:25]([O:28][CH2:32][CH2:33][N:34]3[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]3)=[CH:26][CH:27]=2)=[CH:19][CH:20]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 74826Piperidine, 1-(2-chloroethyl)-, hydrochlorideHCID 189188093,5-dimethyl-2-[4-(4-hydroxybenzoyl)benzylthio]thieno[2,3-d]pyrimidin-4(3H)-one

Produkt 1

HCID 189191603,5-Dimethyl-2-[4-[4-(2-piperidinoethoxy)benzoyl]-benzylthio]thieno[2,3-d]pyrimidin-4(3H)-one hydrochlorideAusbeute 77,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 3,5-dimethyl-2-[4-(4-hydroxybenzoyl)benzylthio]thieno[2,3-d]pyrimidin-4(3H)-one (255 mg), 1-(2-chloroethyl)piperidine hydrochloride (122 mg) and potassium carbonate (250 mg) in DMF (8 ml) was stirred at 60° C. for 15 hours. This reaction mixture was concentrated, the residue was dissolved in ethyl acetate, and the solution was washed with water and dried. Then, HCl/ethyl acetate was added and the precipitated hydrochloride was collected by filtration and dried to provide the title compound as colorless solid (268 mg).

Aufarbeitung

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washthe solution was washed with water
  4. customdried
  5. additionThen, HCl/ethyl acetate was added
  6. filtrationthe precipitated hydrochloride was collected by filtration
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-94b64c856fe94438baf8da1b00e709ec
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05753664

Notizen zur Reaktion

Wird geladen…