Trifluoroacetic acid → 3-(1H-pyrazol-4-yl)-pyridine-2,6-diamine

HRID 77877

Reaktionsgleichung

Reaktionsgleichung von HRID 77877
C([N:20]1[CH:24]=[C:23]([C:25]2[C:26]([NH2:32])=[N:27][C:28]([NH2:31])=[CH:29][CH:30]=2)[CH:22]=[N:21]1)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.FC(F)(F)C(O)=O>C(Cl)Cl>[NH:20]1[CH:24]=[C:23]([C:25]2[C:26]([NH2:32])=[N:27][C:28]([NH2:31])=[CH:29][CH:30]=2)[CH:22]=[N:21]1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 59255416HCID 59255416, Verbindung

Produkt 1

HCID 592551723-(1H-pyrazol-4-yl)-pyridine-2,6-diamineAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 3-(1-trityl-1H-pyrazol-4-yl)-pyridin-2,6-diamine (10.0 g, 25.7 mmol) described in Manufacturing Example 36-1-1 in methylene chloride (14 mL) was added trifluoroacetic acid (7 mL) under nitrogen atmosphere, which was stirred for 1 hour at room temperature. The reaction mixture was concentrated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate, then ethyl acetate:methanol=10:1) to obtain the title compound (600 mg, 60%).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated under a reduced pressure
  2. customThe residue was purified by NH silica gel column chromatography (ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-6ef575f901f14b698e170b2b33a948ff
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08841327B2

Verknüpfte Notizen

Wird geladen…