Methanol → Methyl 3-(dimethylsulfamoyl)benzoate
Reaktionsgleichung
[CH3:1][N:2]([CH3:15])[S:3]([C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][CH:14]=1)[C:9]([OH:11])=[O:10])(=[O:5])=[O:4].S(=O)(=O)(O)O.[CH3:21]O>>[CH3:1][N:2]([CH3:15])[S:3]([C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][CH:14]=1)[C:9]([O:11][CH3:21])=[O:10])(=[O:4])=[O:5]Komponenten
4
Versuchsvorschrift
3-(N,N-Dimethylsulfamoyl)benzoic acid (200 mg, 0.872 mmol) was refluxed overnight in the presence of concentrated sulfuric acid (5.64 mg, 0.044 mmol) in methanol (10 mL) at 70° C. Reaction was monitored by TLC. After completion of the reaction, the solvent was removed by vacuum and then compound was purified by column chromatography affording the title compound (125 mg). 1H NMR (400 MHz, CDCl3): δ 8.42 (s, 1H), 8.27 (d, 1H, J=8.0 Hz), 7.97 (d, 1H, J=7.2 Hz), 7.65 (t, 1H, J=8.0 Hz), 3.96 (s, 3H), 2.74 (s, 6H). ESI-MS: 244.0 [M+H]+.
Aufarbeitung
- customReaction
- customAfter completion of the reaction
- customthe solvent was removed by vacuum
- customcompound was purified by column chromatography
Quellen und Nachweise
- ORD-Eintrag
- ord-df478f5fe3d74dc29b77ac33dd68c4c2
- Quelldatensatz
- uspto-grants-2015_03
- Patentnummer
- US08987335B2
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