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Hydrochloric Acid → HCID 18917249, Verbindung

HRID 5590
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 5590
C1(C)C=CC(S(O[CH2:11][CH2:12][CH:13]2[C:19]3[CH:20]=[C:21]([Cl:24])[CH:22]=[CH:23][C:18]=3[N:17]([C:25](=[O:43])[C:26]3[CH:31]=[CH:30][C:29]([NH:32][C:33](=[O:41])[C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=4[CH3:40])=[CH:28][C:27]=3[CH3:42])[CH2:16][CH2:15][CH2:14]2)(=O)=O)=CC=1.[I-].[Na+].[C:47]([N:50]1[CH2:55][CH2:54][NH:53][CH2:52][CH2:51]1)(=[O:49])[CH3:48].Cl>CN(C)C=O.C(OCC)C>[ClH:24].[C:47]([N:50]1[CH2:55][CH2:54][N:53]([CH2:11][CH2:12][CH:13]2[C:19]3[CH:20]=[C:21]([Cl:24])[CH:22]=[CH:23][C:18]=3[N:17]([C:25](=[O:43])[C:26]3[CH:31]=[CH:30][C:29]([NH:32][C:33](=[O:41])[C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=4[CH3:40])=[CH:28][C:27]=3[CH3:42])[CH2:16][CH2:15][CH2:14]2)[CH2:52][CH2:51]1)(=[O:49])[CH3:48]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 5238Sodium IodideHCID 837951-AcetylpiperazineHCID 189174665-[2-(p-toluenesulfonyloxy)ethyl]-7-chloro-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine

Produkt 1

HCID 18917249HCID 18917249, VerbindungAusbeute 121,5 %

Reagenzien, Katalysatoren, Lösungsmittel

2
HCID 3283Diethyl EtherLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 5-[2-(p-toluenesulfonyloxy)ethyl]-7-chloro-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.25 g) in dry dimethylformamide (20 ml) are added sodium iodide (0.178 g) and 4-acetylpiperazine (0.152 g), and the mixture is stirred at room temperature for one hour. The mixture is heated at 50° C. for 2 hours, and further at 60° C. for 3 hours. To the reaction solution are added 1N-hydrochloric acid and diethyl ether, and the aqueous layer is collected and neutralized with saturated aqueous sodium hydrogen carbonate solution, and extracted with dichloromethane. The dichloromethane layer is washed with water, dried, and the solvent is distilled off. To the resulting residue is added hydrochloric acid/ethanol to give 5-[2-(4-acetyl-1-piperazinyl)ethyl]-7-chloro-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine hydrochloride (150 mg) as colorless amorphous.

Aufarbeitung

  1. temperatureThe mixture is heated at 50° C. for 2 hours
  2. waitfurther at 60° C. for 3 hours
  3. customthe aqueous layer is collected
  4. extractionextracted with dichloromethane
  5. washThe dichloromethane layer is washed with water
  6. customdried
  7. distillationthe solvent is distilled off
  8. additionTo the resulting residue is added hydrochloric acid/ethanol

Quellen und Nachweise

ORD-Eintrag
ord-51fadc04c6db458b83e946b701fe0f2a
Quelldatensatz
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05244898

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