Thionyl Chloride → N-Methyl 4-Methoxybenzimidoyl Chloride
Reaktionsgleichung
[CH3:1][NH:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][CH:5]=1.S(Cl)([Cl:15])=O>>[CH3:1][N:2]=[C:3]([Cl:15])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][CH:5]=1Komponenten
3
Versuchsvorschrift
N-Methyl 4-methoxybenzamide (13.95 g, 84.5 mmole) was placed in a 50 ml round bottom flask equipped with magnetic stirrer, heating mantle, condenser and base trap. Thionyl chloride (33 g, 278 mmole) was added. The reaction was stirred and heated at reflux until gas evolution ceased (three hours). The excess thionyl chloride was distilled at ca. 15 mm Hg, and the product distilled at 75°-80° C. (0.1 mm Hg) to yield 11.9 g (76%) of the title compound as a clear colorless liquid.
Aufarbeitung
- customequipped with magnetic stirrer
- temperatureheating mantle, condenser and base trap
- temperatureheated
- temperatureat reflux until gas evolution
- custom(three hours)
- distillationThe excess thionyl chloride was distilled at ca. 15 mm Hg
- distillationthe product distilled at 75°-80° C. (0.1 mm Hg)
Quellen und Nachweise
- ORD-Eintrag
- ord-4883742856d94c599313418f15ed2269
- Quelldatensatz
- uspto-grants-1985_07
- Patentnummer
- US04528382
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