Reaktionsgleichung
Cl[CH2:2][C:3]1[C:4]([CH3:9])=[N:5][O:6][C:7]=1[CH3:8].[NH3:10]>>[NH2:10][CH2:2][C:3]1[C:4]([CH3:9])=[N:5][O:6][C:7]=1[CH3:8]Komponenten
3
Versuchsvorschrift
4-Chloromethyl-3,5-dimethylisoxazole (700 mg, 4.8 mmol) is suspended in concentrated aqueous ammonia at 20–25 degrees C., and vigorously stirred overnight. The reaction mixture is extracted with isopropyl alcohol/chloroform (10/90, 2×). The combined organic phases are concentrated under nitrogen flow. The residue is purified by flash chromatography methanol/methylene chloride (5–20%, 1% triethylamine) to give the title compound, MR (CDCl3, 300 MHz) delta3.62, 2.37, 2.29, and 1.44.
Aufarbeitung
- customvigorously stirred overnight
- extractionThe reaction mixture is extracted with isopropyl alcohol/chloroform (10/90, 2×)
- concentrationThe combined organic phases are concentrated under nitrogen flow
- customThe residue is purified by flash chromatography methanol/methylene chloride (5–20%, 1% triethylamine)
Quellen und Nachweise
- ORD-Eintrag
- ord-617fd34c1f7440829ca5fc43a8612df5
- Quelldatensatz
- uspto-grants-2007_05
- Patentnummer
- US07214715B2
Verknüpfte Notizen
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