Trifluoroacetic acid → HCID 90407688, Verbindung

HRID 510234Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 510234
[N:1]1([C:6]2[C:7]3[CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][C:8]=3[N:9]=[CH:10][N:11]=2)[CH:5]=[N:4][CH:3]=[N:2]1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH3:1].[N:1]1([C:6]2[C:7]3[CH2:15][CH2:14][NH:13][CH2:12][C:8]=3[N:9]=[CH:10][N:11]=2)[CH:5]=[N:4][CH:3]=[N:2]1

Komponenten

5

Edukt 2

HCID 6422Trifluoroacetic acidHCID 90407776HCID 90407776, Verbindung

Produkt 2

HCID 222AmmoniaHCID 90407688HCID 90407688, VerbindungAusbeute 33 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To the product of Example 110, step a (850 mg, 2.8 mmol) in DCM (14 mL) was added TFA (5 mL). After stirring 2 h, the reaction was concentrated in vacuo. Chromatography on SiO2 eluting with 2 M NH3 in MeOH/DCM afforded the desired product as a pale yellow solid (190 mg, 33%). This material was used without further purification. MS (ESI) mass calcd. C9H10N6, 202.2. m/z found 203.1 [M+H]+. 1H NMR (500 MHz, CDCl3): 8.92 (s, 1H), 8.63 (d, J=1.2 Hz, 1H), 7.85 (d, J=1.2 Hz, 1H), 4.23 (s, 2H), 3.36 (t, J=5.7 Hz, 2H), 3.23 (t, J=5.9 Hz, 2H).

Aufarbeitung

  1. concentrationthe reaction was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-c124cd29ea4b4c2b814323dfadb5217d
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09096596B2

Notizen zur Reaktion

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