反应详情

To a solution of 4-(3-methyl-[1,2,4]thiadiazol-5-yl)-phenylamine (81 mg, 0.42 mmol) in tetrahydrofurane (6.4 mL) was added benzoyl isothiocyanate (76 mg, 0.44 mmol). The reaction was stirred at room temperature for 3 hours. The solvent was removed under reduced pressure and the residue was suspended in methanol (10.6 mL). Potassium carbonate (175 mg, 1.27 mmol) dissolved in water (5.3 mL) was added drop wise to the suspension. The reaction was stirred at room temperature over night. The resulting solution was evaporated and the residue was stirred with water. The precipitate was filtered off, washed with water and with diethyl ether to yield the title compound as a yellow solid (75 mg, 71%). MS ISP (m/e): 251.0 (100) [(M+H)+], 501.1 (83) [(2M+H)+]. 1H NMR (DMSO-D6, 300 MHz): δ (ppm)=10.04 (br s, 1H), 7.94 (d, 2H), 7.72 (d, 2H), 2.63 (s, 3H).

1. customThe solvent was removed under reduced pressure
2. additionwas added drop wise to the suspension
3. stirringThe reaction was stirred at room temperature over night
4. customThe resulting solution was evaporated
5. stirringthe residue was stirred with water
6. filtrationThe precipitate was filtered off
7. washwashed with water and with diethyl ether