Hydrochloric Acid → HCID 178481863, compound

5-Hydroxy-1-methyl-3-trifluoromethylpyrazole (1.7 g (10 mmol)) synthesized in Reference Example 1 and 0.6 g (15 mmol) of sodium hydroxide were dissolved in 10 mL of water. While stirring the resulting solution at room temperature, 1.7 g (20 mmol) of a 35% formalin solution was added dropwise thereto, followed by stirring at the same temperature for 1 hour. Furthermore, 11.0 g (10 mmol) of thiophenol was added dropwise thereto at room temperature, and the obtained mixture was stirred for 7 hours. After the reaction, 5.0 g (50 mmol) of 35% hydrochloric acid was added dropwise thereto, and the precipitated crystal was collected by filtration, washed twice with 5 mL of water and dried by a hot air drier to obtain 2.2 g (yield: 76.4%) of the title compound as a pale yellow crystal. This crystal was recrystallized from n-hexane-2-propanol and obtained as a white crystal.

1. stirringby stirring at the same temperature for 1 hour
2. stirringat room temperature, and the obtained mixture was stirred for 7 hours
3. additionwas added dropwise
4. filtrationthe precipitated crystal was collected by filtration
5. washwashed twice with 5 mL of water
6. customdried by a hot air drier

ORD record

ord-4d11f99a06d949939ba944f1eb4802ad

Source dataset

uspto-grants-2009_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07488831B2