Hydrochloric Acid → HCID 59406948, Verbindung

HRID 80731

Reaktionsgleichung

Reaktionsgleichung von HRID 80731
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]2[N:12]3[N:13]=[C:14]([N:17]4[CH2:21][CH:20]5[CH2:22][N:23](C(OC(C)(C)C)=O)[CH2:24][CH:19]5[CH2:18]4)[CH:15]=[CH:16][C:11]3=[N:10][C:9]=2[C:32]2[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][CH:33]=2)[CH:5]=[CH:4][N:3]=1.Cl>ClCCl>[Cl:38][C:35]1[CH:36]=[CH:37][C:32]([C:9]2[N:10]=[C:11]3[CH:16]=[CH:15][C:14]([N:17]4[CH2:21][CH:20]5[CH:19]([CH2:24][NH:23][CH2:22]5)[CH2:18]4)=[N:13][N:12]3[C:8]=2[C:6]2[CH:5]=[CH:4][N:3]=[C:2]([NH2:1])[CH:7]=2)=[CH:33][CH:34]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 59406953tert-Butyl 5-[3-(2-aminopyrid-4-yl)-2-(4-chlorophenyl)imidazo[1,2-b]pyridazin-6-yl]hexahydropyrrolo[3,4-c]pyrrole-2-carboxylate

Produkt 1

HCID 59406948HCID 59406948, VerbindungAusbeute 72,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 0.16 g (0.29 mmol) of tert-butyl 5-[3-(2-aminopyrid-4-yl)-2-(4-chlorophenyl)imidazo[1,2-b]pyridazin-6-yl]hexahydropyrrolo[3,4-c]pyrrole-2-carboxylate in 3 mL of dichloromethane are added 1.5 mL (18 mmol) of concentrated hydrochloric acid. After stirring for 1 hour 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 0.091 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-da7ce3c1c6e449a6b35a16527eb920d4
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846676B2

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