1,4-Dioxane → HCID 46203865, Verbindung

HRID 1724870Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1724870
[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([NH2:9])[CH:5]=[CH:4][N:3]=1.C([O-])(O)=O.[Na+].O1CCOCC1.Br.Br[CH2:23][C:24]([C:26]1[C:31]([C:32]([F:35])([F:34])[F:33])=[CH:30][CH:29]=[CH:28][N:27]=1)=O>O>[F:35][C:32]([F:33])([F:34])[C:31]1[C:26]([C:24]2[N:1]=[C:2]3[N:3]=[CH:4][CH:5]=[C:6]([NH2:9])[C:7]3=[N:8][CH:23]=2)=[N:27][CH:28]=[CH:29][CH:30]=1

Komponenten

6

Edukt 4

HCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 22135565Pyridine-2,3,4-triamineHCID 462042022-Bromo-1-(3-trifluoromethyl-pyridin-2-yl)-ethanone hydrobromide

Produkt 1

HCID 46203865HCID 46203865, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Dissolve 2,3,4-triaminopyridine (2.5 mmol) in water (20 mL). Add NaHCO3 (0.63 g, 7.5 mmol), dioxane (10 mL), and 2-bromo-1-(3-trifluoromethyl-pyridin-2-yl)-ethanone hydrobromide (0.5 g) and stir at 100° C. for 2 hours. Cool the mixture and extract with EtOAc (4×10 mL). Wash the combined organic extracts with brine and dry over Na2SO4. Purify the residue by preparative HPLC to give the title compound.

Aufarbeitung

  1. temperatureCool the mixture
  2. extractionextract with EtOAc (4×10 mL)
  3. washWash the combined organic extracts with brine
  4. dry with materialdry over Na2SO4
  5. customPurify the residue by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-61395ab9d01848f297c221b3f716704d
Quelldatensatz
uspto-grants-2009_02
Patentnummer
US07488740B2

Notizen zur Reaktion

Wird geladen…