Hydrochloric Acid → HCID 68441414, compound

In a 25-ml eggplant flask provided with a magnetic stirrer was placed 3.3 g (9.3 mmol) of 5-(5-amino-3-trifluoromethyl-1H-1,2,4-triazol-1-yl)-2,4-dimethylbenzenesulfonyl chloride, followed by addition of 3.27 g (50 mmol) of zinc, 10 ml of ethanol and 5 ml (50 mmol) of 35% hydrochloric acid. The mixture was stirred at room temperature for 15 minutes. Then, the mixture was refluxed with heating, for 3 hours. The mixture was cooled to room temperature. Thereto were added 30 ml of water and 30 ml of ethyl acetate to give rise to phase separation. The aqueous phase was extracted with 30 ml of ethyl acetate. The ethyl acetate phase was washed with water and then with a saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate. Vacuum distillation was conducted to distill off ethyl acetate to obtain a title compound as 1.9 g of oil. Yield: 71%

1. customIn a 25-ml eggplant flask provided with a magnetic stirrer
2. temperatureThen, the mixture was refluxed
3. temperaturewith heating, for 3 hours
4. temperatureThe mixture was cooled to room temperature
5. customto give rise
6. customto phase separation
7. extractionThe aqueous phase was extracted with 30 ml of ethyl acetate
8. washThe ethyl acetate phase was washed with water
9. dry with materialwith a saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate
10. distillationVacuum distillation
11. distillationto distill off ethyl acetate

ORD record

ord-aec2467916e94e8dba02c90a95bdd84e

Source dataset

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08440838B2