Hydrochloric Acid → 4-[6-Chloro-2-(4-chlorophenyl)imidazo[1,2-b]pyridazin-3-yl]pyrid-2-ylamine

HRID 1803895Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1803895
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8]([C:18]3[CH:23]=[CH:22][N:21]=[C:20]([NH:24]C(=O)OC(C)(C)C)[CH:19]=3)=[C:9]([C:11]3[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=3)[N:10]=2)[N:7]=1.Cl>ClCCl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8]([C:18]3[CH:23]=[CH:22][N:21]=[C:20]([NH2:24])[CH:19]=3)=[C:9]([C:11]3[CH:12]=[CH:13][C:14]([Cl:17])=[CH:15][CH:16]=3)[N:10]=2)[N:7]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 59406969tert-Butyl {4-[6-chloro-2-(4-chlorophenyl)imidazo[1,2-b]pyridazin-3-yl]pyrid-2-yl}carbamate

Produkt 1

HCID 594069504-[6-Chloro-2-(4-chlorophenyl)imidazo[1,2-b]pyridazin-3-yl]pyrid-2-ylamineAusbeute 94,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a suspension of 0.76 g (1.67 mmol) of tert-butyl {4-[6-chloro-2-(4-chlorophenyl)imidazo[1,2-b]pyridazin-3-yl]pyrid-2-yl}carbamate in 8 mL of dichloromethane are added 4 mL (48 mmol) of hydrochloric acid. After stirring for 2 hours at room temperature, the solvent is evaporated off under reduced pressure, the oily residue is taken up with aqueous ammonia and the product is extracted with dichloromethane. The organic phase is filtered on a hydrophobic cartridge and concentrated under reduced pressure. The solid obtained is triturated with diisopropyl ether to give 0.56 g of solid after filtering off and drying under reduced pressure.

Aufarbeitung

  1. customthe solvent is evaporated off under reduced pressure
  2. extractionthe product is extracted with dichloromethane
  3. filtrationThe organic phase is filtered on a hydrophobic cartridge
  4. concentrationconcentrated under reduced pressure
  5. customThe solid obtained
  6. customis triturated with diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-c342952c3af145e49a8ac838e6834eb1
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08354405B2

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