Reaktionsgleichung
[F:1][C:2]([F:24])([F:23])[O:3][C:4]1[CH:5]=[C:6]([C:10]2[C:14]3[CH:15]=[C:16]([C:19]([NH:21][NH2:22])=[O:20])[CH:17]=[CH:18][C:13]=3[O:12][CH:11]=2)[CH:7]=[CH:8][CH:9]=1.[Cl:25][CH2:26][C:27](OC)(OC)OC>>[Cl:25][CH2:26][C:27]1[O:20][C:19]([C:16]2[CH:17]=[CH:18][C:13]3[O:12][CH:11]=[C:10]([C:6]4[CH:7]=[CH:8][CH:9]=[C:4]([O:3][C:2]([F:23])([F:1])[F:24])[CH:5]=4)[C:14]=3[CH:15]=2)=[N:21][N:22]=1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
A mixture of 3-[3-(trifluoromethoxy)phenyl]-1-benzofuran-5-carbohydrazide (3.00 g, 8.92 mmol) and 2-chloro-1,1,1-trimethoxyethane (4.70 mL, 24.4 mmol) was stirred at 80° C. for 3 hr. The reaction mixture was purified by silica gel column chromatography (hexane/ethyl acetate=1/1) and recrystallized from hexane/ethyl acetate to give the title compound (2.39 g, yield 68%) as colorless crystals.
Aufarbeitung
- customThe reaction mixture was purified by silica gel column chromatography (hexane/ethyl acetate=1/1)
- customrecrystallized from hexane/ethyl acetate
Quellen und Nachweise
- ORD-Eintrag
- ord-c35c8c783b434e2daf29d1b04cd3c2f2
- Quelldatensatz
- uspto-grants-2013_07
- Patentnummer
- US08492378B2
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