Reaktionsgleichung
[C:1]1([CH:7]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[O:8][CH:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH:16]([OH:19])[CH2:17][NH2:18])[CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:27]1[CH:28]=[CH:29][C:30]2[N:31]([N:33]=[CH:34][N:35]=2)[N:32]=1.C(=O)(O)[O-].[Na+]>>[C:20]1([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[O:8][CH:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH:16]([OH:19])[CH2:17][NH:18][C:27]3[CH:28]=[CH:29][C:30]4[N:31]([N:33]=[CH:34][N:35]=4)[N:32]=3)[CH2:11][CH2:10]2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1Komponenten
4
Versuchsvorschrift
0.675 g of 3-[4-(diphenylmethoxy)piperidino]-2-hydroxypropylamine and 0.335 g of 6-chloro[1,2,4]triazolo [1,5-b]pyridazine were stirred at 135-140° C. for 3 hours. After cooling, aqueous sodium bicarbonate was added, followed by extraction with ethyl acetate-tetrahydrofuran (2:1); the extract was washed with saline and dried with sodium sulfate. The dry product was concentrated under reduced pressure; the residue was subjected to silica gel column chromatography and eluted with ethyl acetate:methanol:triethylamine (90:10:1). The desired fraction was collected, recrystallized from ethyl acetate and dried to yield 0.509 g of the title compound.
Aufarbeitung
- temperatureAfter cooling
- extractionfollowed by extraction with ethyl acetate-tetrahydrofuran (2:1)
- washthe extract was washed with saline
- dry with materialdried with sodium sulfate
- concentrationThe dry product was concentrated under reduced pressure
- washeluted with ethyl acetate:methanol:triethylamine (90:10:1)
- customThe desired fraction was collected
- customrecrystallized from ethyl acetate
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-134a977e4c4e49b18d1d70faa17616d6
- Quelldatensatz
- uspto-grants-2001_06
- Patentnummer
- US06248740B1
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