80087-71-4

75-15-0

61272-76-2

80087-71-4

At room temperature and under the protection of argon, 2-iodo-4-fluoroaniline (2 mmol), carbon disulfide (10 mmol), sodium sulfide (4 mmol), and N,N-dimethylformamide (2 mL) were sequentially added to a 50 mL sealed reaction tube, and the air inside the reaction tube was replaced three times with argon. The reaction tube was sealed and placed in an oil bath at 110°C with electromagnetic stirring for 12 hours. The reaction process was monitored by thin layer chromatography (TLC, silica gel plate). Upon completion of the reaction, the reaction mixture was cooled to room temperature, 3 mol/L hydrochloric acid (2 mL) was added slowly and stirring was continued for 30 min. Subsequently, the reaction mixture was extracted with dichloromethane (3 x 20 mL), the organic phases were combined and dried with anhydrous magnesium sulfate. After the solvent was removed by concentration under reduced pressure, the residue was purified by silica gel column chromatography (eluent: petroleum ether/ethyl acetate gradient elution) to afford the target compound 6-fluoro-2-mercaptobenzothiazole.