Hydrochloric Acid → HCID 178516408, Verbindung

HRID 1724840Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1724840
Cl[C:2]1[C:11]2[C:6](=[N:7][C:8]([C:12]3[C:17]([C:18]([F:21])([F:20])[F:19])=[CH:16][CH:15]=[CH:14][N:13]=3)=[CH:9][CH:10]=2)[N:5]=[C:4]([O:22]C)[CH:3]=1.[F:24][C:25]([F:34])([F:33])[C:26]1[CH:32]=[CH:31][C:29]([NH2:30])=[CH:28][CH:27]=1.Cl.CCOCC>C(O)(C)C>[F:24][C:25]([F:33])([F:34])[C:26]1[CH:27]=[CH:28][C:29]([NH:30][C:2]2[C:11]3[C:6](=[N:7][C:8]([C:12]4[C:17]([C:18]([F:21])([F:20])[F:19])=[CH:16][CH:15]=[CH:14][N:13]=4)=[CH:9][CH:10]=3)[N:5]=[C:4]([OH:22])[CH:3]=2)=[CH:31][CH:32]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 99644-(Trifluoromethyl)anilineHCID 575611334-Chloro-2-methoxy-7-[3-(trifluoromethyl)pyridin-2-yl]-1,8-naphthyridine

Produkt 1

HCID 178516408HCID 178516408, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

Heat 4-chloro-2-methoxy-7-(3-trifluoromethyl-pyridin-2-yl)-[1,8]naphthyridine (600 mg, 1.8 mmol), 4-trifluoromethylaniline (322 mg, 2.0 mmol) and 2M hydrochloric acid in ether (1 mL, 2.0 mmol) in isopropanol (15 mL) at 80° C. for 16 hours. Cool the mixture and collect the precipitate by filtration. Partition the solid between ethyl acetate and saturated sodium bicarbonate solution. Separate the layers and extract the aqueous layer with further ethyl acetate. Wash the combined organic extracts with brine, dry (MgSO4) and evaporate to give the title compound.

Aufarbeitung

  1. temperatureCool the mixture
  2. customcollect the precipitate
  3. filtrationby filtration
  4. customPartition the solid between ethyl acetate and saturated sodium bicarbonate solution
  5. customSeparate the layers
  6. extractionextract the aqueous layer with further ethyl acetate
  7. washWash the combined organic extracts with brine
  8. dry with materialdry (MgSO4)
  9. customevaporate

Quellen und Nachweise

ORD-Eintrag
ord-934bf16faf4b46f1882845998c4add96
Quelldatensatz
uspto-grants-2009_02
Patentnummer
US07488740B2

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