Ethyl isocyanate → HCID 59603083, Verbindung
Reaktionsgleichung
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([NH2:10])=[N:7][C:6]=2[CH:11]=1.[CH2:12]([N:14]=[C:15]=[O:16])[CH3:13]>O1CCOCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([NH:10][C:15]([NH:14][CH2:12][CH3:13])=[O:16])=[N:7][C:6]=2[CH:11]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 79 °C
Versuchsvorschrift
To a suspension of 5-bromo-benzothiazol-2-ylamine IV (0.23 g, 1.0 mmol) in 1,4-dioxane (10 mL) was added ethylisocyanate (0.36 g, 0.38 mL, 5.02 mmol). The reaction mixture was heated up to 78-80° C. overnight. After completion of reaction (TLC monitoring), 1,4-dioxane was distilled off and co evaporated with hexane. The resulting solid was treated with water to 60-70° C. for 3-5 h. The resulting solid was filtered off and again washed with hot water, dried under high vacuum to obtain the desired product as off-white solid (0.15 g, 50%). 1H NMR (DMSO-d6, 400 MHz): δ 1.08 (t, J=7.20 Hz, 3H), 3.18 (m, 2H), 6.70 (br s, 1H), 7.36 (dd, J=1.60 and 8.0 Hz, 1H), 7.79 (d, J=1.60 Hz, 1H), 7.84 (d, J=8.40 Hz, 1H) and 10.85 (br s, 1H). MS: 300.07 (M+H+).