Diethyl Ether → 1-(4-Methyl-1,2,3-thiadiazol-5-yl)ethan-1-one
Reaktionsgleichung
CON(C)[C:4]([C:6]1[S:10][N:9]=[N:8][C:7]=1[CH3:11])=[O:5].[CH2:13](OCC)C.C[Mg]I>C1COCC1>[C:4]([C:6]1[S:10][N:9]=[N:8][C:7]=1[CH3:11])(=[O:5])[CH3:13]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a solution of N-methoxy-N-methyl-4-methyl-1,2,3-thiadiazole-5-carboxamide (11.31 g, 60.4 mmol) in THF (100 ml) was added 2M diethyl ether solution of methylmagnesium iodide (45.3 ml, 90.6 mmol) over 0.5 h at 0° C. The mixture was allowed to warm to room temperature and stirred for 3 h. The mixture was quenched with saturated aqueous ammonium chloride (100 ml) and then extracted with diethyl ether (200 ml×2). The extracts were dried (MgSO4) and concentrated to give 7.49 g (87%) of the title compound as a pale brown oil.
Aufarbeitung
- customThe mixture was quenched with saturated aqueous ammonium chloride (100 ml)
- extractionextracted with diethyl ether (200 ml×2)
- dry with materialThe extracts were dried (MgSO4)
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-8c8839183b754a71ad88b973b7d40d88
- Quelldatensatz
- uspto-grants-2003_08
- Patentnummer
- US06608070B1
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