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Ammonia → HCID 18968908, Verbindung

HRID 398790
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 398790
Cl.[NH2:2][CH:3]1[C:9](=[O:10])[NH:8][C:7]2[CH:11]=[CH:12][C:13]3[C:18]([C:6]=2[CH2:5][CH2:4]1)=[CH:17][CH:16]=[CH:15][CH:14]=3.N>O>[NH2:2][CH:3]1[C:9](=[O:10])[NH:8][C:7]2[CH:11]=[CH:12][C:13]3[C:18]([C:6]=2[CH2:5][CH2:4]1)=[CH:17][CH:16]=[CH:15][CH:14]=3
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 18968915HCID 18968915, Verbindung

Produkt 1

HCID 18968908HCID 18968908, VerbindungAusbeute 97,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of 3-azido-4-oxo-2,3,4,5-tetrahydro-1H-naphtho-[2,1-b]azepine (16.0 g, 63.4 mmol) in a mixture of dry dioxane (150 ml) and ethanol (150 ml), palladium on carbon (10%, 2 g) was added. This mixture was hydrogenated under a pressure of 5 bar and with efficient stirring for 24 h. The reaction mixture was filtered and excess hydrogenchloride in ethanol was added. The precipitated solid was isolated, washed with ethanol and dried to give 14.4 g of 3-amino-4-oxo-2,3,4,5-tetrahydro-1H-naphtho[2,1-b]azepine hydrochloride. The above hydrochloride (14.2 g) was dissolved into water (800 ml) by warming. A 25% aqueous ammonia solution was added and a precipitate was formed. The solid was isolated by filtration, washed with water and dried in vacuo to give 11.9 g of 3-amino-4-oxo-2,3,4,5-tetrahydro-1H-naphtho[2,1-b]azepine.

Aufarbeitung

  1. temperatureby warming
  2. customa precipitate was formed
  3. customThe solid was isolated by filtration
  4. washwashed with water
  5. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e1b24c1230fa4921b11737de325bd374
Quelldatensatz
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05817654

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