1,2-Dichloroethane → HCID 178513834, Verbindung

HRID 222005

Reaktionsgleichung

Reaktionsgleichung von HRID 222005
[NH:1]([C:3]1[CH:4]=[CH:5][C:6]2[C:7]([N:19]=1)=[N:8][C:9]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[C:10]([OH:12])[N:11]=2)[NH2:2].C1C=CC2N(O)N=NC=2C=1.[C:30](O)(=O)[C:31]([NH2:33])=[O:32].C(Cl)CCl.C(O)(C(F)(F)F)=O>CN1C(=O)CCC1.O>[OH:12][C:10]1[N:11]=[C:6]2[CH:5]=[CH:4][C:3]3=[N:1][N:2]=[C:30]([C:31]([NH2:33])=[O:32])[N:19]3[C:7]2=[N:8][C:9]=1[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

Komponenten

8

Edukt 5

HCID 111,2-DichloroethaneHCID 974Oxamic AcidHCID 6422Trifluoroacetic acidHCID 757711-HydroxybenzotriazoleHCID 178514300HCID 178514300, Verbindung

Produkt 1

HCID 178513834HCID 178513834, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

To a mixture of 6-hydrazinyl-3-phenylpyrido[2,3-b]pyrazin-2(1H)-one (3-3) (300 mg, 1.19 mmol), HOBt (218 mg, 1.42 mmol) and oxamic acid (130 mg, 1.42 mmol) in NMP (12 mL) was added EDC (272 mg, 1.42 mmol) at room temperature and the mixture was stirred for 30 min. After addition of TFA (0.091 mL, 1.19 mmol), the mixture was heated under microwave irradiation at 150° C. for 30 minutes. To a mixture was added water (60 mL) and the precipitate was collected by filtration to give 3-hydroxy-2-phenyl[1,2,4]triazolo[4′,3′:1,6]pyrido[2,3-b]pyrazin-9-carboxamide (9-1) as a yellow powder.

Aufarbeitung

  1. filtrationthe precipitate was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-66a85126e86f4012a368f42eb2537669
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08207169B2

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