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Sodium Hydroxide → HCID 9867305, Verbindung

HRID 2226113
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2226113
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:22]3[CH:23]=[C:24]([O:29][CH3:30])[C:25]([O:27][CH3:28])=[CH:26][C:21]=3[C@H:20]3[C@H:15]([CH2:16][CH2:17][N:18]([CH3:31])[CH2:19]3)[N:14]=2)=[CH:9][CH:8]=1.[OH-].[Na+]>O1CCOCC1.N1C=CC=CC=1>[CH3:30][O:29][C:24]1[C:25]([O:27][CH3:28])=[CH:26][C:21]2[C@H:20]3[C@H:15]([CH2:16][CH2:17][N:18]([CH3:31])[CH2:19]3)[N:14]=[C:13]([C:10]3[CH:11]=[CH:12][C:7]([NH:6][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:8][CH:9]=3)[C:22]=2[CH:23]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 31297Methanesulfonyl chlorideHCID 86733645HCID 86733645, Verbindung

Produkt 1

HCID 9867305HCID 9867305, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittelHCID 31275
1,4-Dioxane
Lösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A solution of 0.6 ml methanesulphonyl chloride in 3 ml absolute dioxane is added dropwise to a solution of 2.1 g rac-cis-6-(4-aminophenyl)-8,9-dimethoxy-1,2,3,4,4a, 10b-hexahydro-2-methyl-benzo[c ][1,6]naphthyridine in 20 ml absolute pyridine, and the mixture is then stirred at 60° C. for a further 3 h. After cooling, the mixture is poured onto 100 ml of an ice/water mixture, rendered alkaline with dilute sodium hydroxide solution and extracted with n-butanol. After the n-butanol has been evaporated off, the residue which remains is extracted with methylene chloride and the organic phase is dried over sodium sulphate and then concentrated. 2.4 g of the title compound are obtained as the residue and are converted into the dihydrochloride with ethereal HCl, and the product is recrystallized from non-dried methanol. Yield: 2.3 g of the title compound as the dihydrochloride hydrate. M.p. 239°-240° C. (decomposition).

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionextracted with n-butanol
  3. customAfter the n-butanol has been evaporated off
  4. extractionthe residue which remains is extracted with methylene chloride
  5. dry with materialthe organic phase is dried over sodium sulphate
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-be0c0c4e80dd42fc8863e4aa3dd0e8e4
Quelldatensatz
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05346904

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