HCID 23002992, Verbindung → 7-Chloro-8-morpholin-4-yl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine monohydrobromide

HRID 1692607Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1692607
[Cl:1][C:2]1[C:12]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)=[N:11][C:10]2[O:9][CH2:8][CH2:7][N:6](C(OC(C)(C)C)=O)[CH2:5][C:4]=2[CH:3]=1.[BrH:26].C(O)C>C(O)C>[BrH:26].[Cl:1][C:2]1[C:12]([N:13]2[CH2:14][CH2:15][O:16][CH2:17][CH2:18]2)=[N:11][C:10]2[O:9][CH2:8][CH2:7][NH:6][CH2:5][C:4]=2[CH:3]=1

Komponenten

4

Edukt 2

HCID 23002992HCID 23002992, VerbindungHCID 67279788tert-butyl 7-chloro-8-morpholin-4-yl-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate

Produkt 1

HCID 672802287-Chloro-8-morpholin-4-yl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine monohydrobromideAusbeute 25 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of the compound (0.10 g) obtained in step 1 in ethanol (1 mL) was added hydrobromic acid-ethanol solution (1 mL), and the mixture was stirred at room temperature for 4 hr. The solvent was evaporated under reduced pressure, and the aqueous layer was made basic with ethyl acetate and aqueous sodium hydroxide solution. The organic layer was washed with brine and dried, and the solvent was evaporated under reduced pressure. Ethyl acetate was added to the residue, and hydrobromic acid-ethanol solution was added. The precipitate was collected by filtration to give the title compound (0.03 g, 25%) as a white powder.

Aufarbeitung

  1. customThe solvent was evaporated under reduced pressure
  2. washThe organic layer was washed with brine
  3. customdried
  4. customthe solvent was evaporated under reduced pressure
  5. additionEthyl acetate was added to the residue, and hydrobromic acid-ethanol solution
  6. additionwas added
  7. filtrationThe precipitate was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-46e55518a98a4a57b21a3df181202d8b
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08158617B2

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