Ethyl trifluoroacetate → HCID 67387617, compound

Temperature

0 °C

First, 1.8 g of ethyl trifluoroacetate and 50 mL of 1-butanol were put in a three-neck flask, and the air in the flask was replaced by nitrogen. After that, the mixture was stirred at 0° C. for 10 minutes, and 0.397 g of hydrazine monohydrate was dripped to the mixed solution. This mixed solution was stirred at 0° C. for 20 minutes, and then stirred at room temperature for 1 hour to be reacted. After the reaction, 3.0 g of N-[(ethylsulfanyl)phenylmethylidene]aniline was further added to the mixed solution, and the solution was heated and stirred at 120° C. for 5 hours to be reacted. The mixed solution after the reaction was cooled down to room temperature and filtered, so that filtrate was obtained. The obtained filtrate was concentrated to give a solid. This solid was washed with hexane, so that the triazole derivative HCF3ptz was prepared (yield: 26%). The synthesis scheme of Step 1 is shown by (a-2).

1. stirringThis mixed solution was stirred at 0° C. for 20 minutes
2. stirringstirred at room temperature for 1 hour
3. customto be reacted
4. additionwas further added to the mixed solution
5. temperaturethe solution was heated
6. stirringstirred at 120° C. for 5 hours
7. customto be reacted
8. temperatureThe mixed solution after the reaction was cooled down to room temperature
9. filtrationfiltered, so that filtrate
10. customwas obtained
11. concentrationThe obtained filtrate was concentrated
12. customto give a solid
13. washThis solid was washed with hexane, so that the triazole derivative HCF3ptz
14. customwas prepared (yield: 26%)
15. customThe synthesis scheme of Step 1

ORD record

ord-b70c02b5970048e48da12860c0563424

Source dataset

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09005773B2