Sodium Carbonate → HCID 20371485, Verbindung

HRID 616220

Reaktionsgleichung

Reaktionsgleichung von HRID 616220
C(=O)([O-])[O-].[Na+].[Na+].[CH:7]1[C:17]2[CH2:16][CH2:15][C:14]3[CH:18]=[CH:19][CH:20]=[CH:21][C:13]=3[C:12](=[C:22]3[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]3)[C:11]=2[CH:10]=[CH:9][CH:8]=1.Br[CH2:29][CH2:30][CH2:31][C:32](=[O:34])[CH3:33]>C(Cl)(Cl)Cl>[CH:7]1[C:17]2[CH2:16][CH2:15][C:14]3[CH:18]=[CH:19][CH:20]=[CH:21][C:13]=3[C:12](=[C:22]3[CH2:23][CH2:24][N:25]([CH2:29][CH2:30][CH2:31][C:32](=[O:34])[CH3:33])[CH2:26][CH2:27]3)[C:11]=2[CH:10]=[CH:9][CH:8]=1

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 774932-Pentanone, 5-bromo-HCID 1201458Desloratadine impurity 24

Produkt 1

HCID 20371485HCID 20371485, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

9.2 g of sodium carbonate are added to a solution of 10 g of 4-(10,11-dihydro-5-dibenzo[a,d]cycloheptenylidene)piperidine in 100 cc of chloroform, a solution of 7.2 g of 5-bromo-2-pentanone in 50 cc of chloroform is then added dropwise within 20 minutes, and the mixture is subsequently boiled at reflux for 17 hours. After cooling, the precipitate is filtered off, the filtrate is extracted twice with water, dried over magnesium sulphate and concentrated by evaporation. The residue is filtered over a column of 170 g of silica gel. The fraction eluted with chloroform containing 1% of methanol is dissolved in acetone and acidifed with hydrogen chloride in ether. After the addition of more ether, the hydrochloride of the title compound crystallizes. M.P. 235°-238°.

Aufarbeitung

  1. temperatureat reflux for 17 hours
  2. temperatureAfter cooling
  3. filtrationthe precipitate is filtered off
  4. extractionthe filtrate is extracted twice with water
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated by evaporation
  7. filtrationThe residue is filtered over a column of 170 g of silica gel
  8. washThe fraction eluted with chloroform containing 1% of methanol
  9. dissolutionis dissolved in acetone
  10. additionAfter the addition of more ether
  11. customthe hydrochloride of the title compound crystallizes

Quellen und Nachweise

ORD-Eintrag
ord-3373ca92e5484e05bbc60f90bbe439f1
Quelldatensatz
uspto-grants-1978_02
Patentnummer
US04072756

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