Potassium Hydroxide → HCID 10913596, Verbindung

HRID 1264563Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1264563
[Cl:1][C:2]1[N:11]2[C:5]([C:6](=[C:16]3[CH2:21][CH2:20][N:19](C(OCC)=O)[CH2:18][CH2:17]3)[C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH2:9][CH2:10]2)=[N:4][CH:3]=1.[OH-].[K+]>C(O)(C)C>[Cl:1][C:2]1[N:11]2[C:5]([C:6](=[C:16]3[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)[C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH2:9][CH2:10]2)=[N:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 14797Potassium HydroxideHCID 18612501HCID 18612501, Verbindung

Produkt 1

HCID 10913596HCID 10913596, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

A mixture of intermediate 12 (30.4 g) and potassium hydroxide (46 g) in isopropanol (370 ml) was stirred and refluxed for 6 hours. The solvent was evaporated. The residue was taken up in water and extracted with DCM. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated. The residue was crystallized from ACN. The precipitate was filtered off and dried, yielding 1.65 g (90%) of 3-chloro-6,11-dihydro-11-(4-piperidinylidene)-5H-imidazo[2,1-b][3]benzazepine (intermediate 13).

Aufarbeitung

  1. temperaturerefluxed for 6 hours
  2. customThe solvent was evaporated
  3. extractionextracted with DCM
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent was evaporated
  8. customThe residue was crystallized from ACN
  9. filtrationThe precipitate was filtered off
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-de9550cbafba4e248c8fa6f863a27025
Quelldatensatz
uspto-grants-2003_04
Patentnummer
US06544979B1

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