Tert-Butyl nitrite → 3-Methyl-5H-6-thia-4,5-diaza-chrysene 6,6-dioxide
Reaktionsgleichung
N[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8]([NH:11][C:12]1[CH:13]=[CH:14][CH:15]=[C:16]2[C:21]=1[N:20]=[C:19]([CH3:22])[CH:18]=[CH:17]2)(=[O:10])=[O:9].C(ON=O)(C)(C)C>C(O)(=O)C>[CH3:22][C:19]1[CH:18]=[CH:17][C:16]2[C:21]([N:20]=1)=[C:12]1[C:13]([C:4]3[C:3]([S:8](=[O:10])(=[O:9])[NH:11]1)=[CH:2][CH:7]=[CH:6][CH:5]=3)=[CH:14][CH:15]=2Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 10 °C
Versuchsvorschrift
2-Amino-N-(2-methyl-quinolin-8-yl)-benzenesulfonamide (Example Compound 15) (164 mg, 0.52 mmol) was suspended in acetic acid (3 ml) and cooled to 10° C. Tert-butylnitrite (93 μl, 0.79 mmol) was added and the reaction was slowly warmed to room temperature over 1 h. The reaction was then quenched with water (4 ml) and the resulting solution was concentrated in vacuo. The crude residue was purified by column chromatography with DCM as the eluent to give the title compound (7 mg, 5%).
Aufarbeitung
- temperaturethe reaction was slowly warmed to room temperature over 1 h
- customThe reaction was then quenched with water (4 ml)
- concentrationthe resulting solution was concentrated in vacuo
- customThe crude residue was purified by column chromatography with DCM as the eluent
Quellen und Nachweise
- ORD-Eintrag
- ord-b30dafd11cc6483bb1736c3326b9b700
- Quelldatensatz
- uspto-grants-2015_08
- Patentnummer
- US09102688B2
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