Anisole → HCID 178470514, Verbindung

HRID 1794683Notizen

Reaktionsgleichung

C1(OC)C=CC=CC=1.COC1C=CC(C[N:16]2[C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[C:19]([C:26](=[O:40])[C:27]3[CH:32]=[C:31]([O:33][CH3:34])[C:30]([O:35][CH3:36])=[CH:29][C:28]=3[N+:37]([O-:39])=[O:38])[N:18]=[N:17]2)=CC=1.COC1C=CC(CN2C(C(=O)C3C=C(OC)C(OC)=CC=3[N+]([O-])=O)=C(C(OCC)=O)N=N2)=CC=1>FC(F)(F)C(O)=O>[CH3:36][O:35][C:30]1[C:31]([O:33][CH3:34])=[CH:32][C:27]([C:26]([C:19]2[NH:18][N:17]=[N:16][C:20]=2[C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:40])=[C:28]([N+:37]([O-:39])=[O:38])[CH:29]=1

Komponenten

Reaktionsbedingungen

Temperatur: 60 °C

Versuchsvorschrift

Anisole (1 ml) was added to a solution of an about 1:1 mixture (4.4 g) of ethyl 1-(4-methoxybenzyl)-4-(4,5-dimethoxy-2-nitrobenzoyl)-1H-1,2,3-triazole-5-carboxylate (Synthesis Example 1, b-1) and ethyl 1-(4-methoxybenzyl)-5-(4,5-dimethoxy-2-nitrobenzoyl)-1H-1,2,3-triazole-4-carboxylate(Synthesis Example 1, b-2) in trifluoroacetic acid (10 ml), and the mixture was stirred at 60° C. for 10 hr. After the mixture was allowed to stand for cooling, the solvent was evaporated under reduced pressure, followed by azeotropic evaporation using toluene. The resultant crystal was collected by filtration, washed with diethyl ether, and then dried to give ethyl 5-(4,5-dimethoxy-2-nitrobenzoyl)-1H-1,2,3-triazole-4-carboxylate (3.12 g, 95%).

Aufarbeitung

temperaturefor cooling
customthe solvent was evaporated under reduced pressure
customfollowed by azeotropic evaporation
filtrationThe resultant crystal was collected by filtration
washwashed with diethyl ether
customdried

Quellen und Nachweise

ORD-Eintrag: ord-45f272dfcf1c4f3aaa16b9d43e8b97cc
Quelldatensatz: uspto-grants-2006_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07022860B2

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