Hydrochloric Acid → HCID 178482540, Verbindung

HRID 493695

Reaktionsgleichung

Reaktionsgleichung von HRID 493695
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([CH2:15][CH2:16][C:17]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)=[O:18])(=[O:14])=[O:13])[CH:6]=[CH:5]2.Cl.[Cl:26][CH2:27][C:28]1[N:29]([CH3:35])/[C:30](=[N:33]/[CH3:34])/[S:31][CH:32]=1.C(=O)([O-])[O-].[K+].[K+].Cl>CN(C=O)C.C(OCC)(=O)C.CCOCC>[ClH:1].[ClH:26].[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([CH2:15][CH2:16][C:17]([N:19]1[CH2:20][CH2:21][N:22]([CH2:27][C:28]3[N:29]([CH3:35])/[C:30](=[N:33]/[CH3:34])/[S:31][CH:32]=3)[CH2:23][CH2:24]1)=[O:18])(=[O:14])=[O:13])[CH:6]=[CH:5]2

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 231308831-(3-((6-Chloro-2-naphthyl)sulfonyl)propionyl)piperazineHCID 178482537HCID 178482537, Verbindung

Produkt 1

HCID 178482540HCID 178482540, VerbindungAusbeute 121,4 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 3283Diethyl EtherLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A suspension of 1-(3-((6-chloro-2-naphthyl)sulfonyl)propionyl)piperazine (2.5 g) obtained in Example 3a), N-((2Z)-4-chloromethyl-3-methyl-1,3-thiazol-2(3H)-ylidene)-N-methylamine hydrochloride (2.2 g) and potassium carbonate (2.4 g) in DMF (50 mL) was mixed at 65° C. for 3 hours. The solvent was distilled off under reduced pressure, the residue was diluted with an aqueous potassium carbonate solution, and extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The product, which was obtained by the purification of the residue with a basic silica gel column, was dissolved in ethyl acetate. A solution of hydrogen chloride in ether was added thereto, and the mixture was concentrated and dried to give the title compound (2.4 g) as a colorless powder.

Aufarbeitung

  1. additionwas mixed at 65° C. for 3 hours
  2. distillationThe solvent was distilled off under reduced pressure
  3. additionthe residue was diluted with an aqueous potassium carbonate solution
  4. extractionextracted with chloroform
  5. dry with materialThe extract was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe product, which was obtained by the purification of the residue with a basic silica gel column
  8. concentrationthe mixture was concentrated
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-3a3fbf0254c84df7ae80a04ae775c56e
Quelldatensatz
uspto-grants-2009_05
Patentnummer
US07534887B2

Verknüpfte Notizen

Wird geladen…