Water → HCID 23075700, compound

To 1.7 g (8.8 mmol) of 5-hydroxy-1-methyl-3-trifluoromethyl-1H-pyrazole in 20 ml of tetrahydrofuran were added 2.5 g (43.8 mmol) of powdery potassium hydroxide and 0.14 g (0.44 mmol) of tetrabutylammonium bromide at room temperature, followed by stirring. Furthermore, chlorodifluoromethane was introduced into the reaction solution until the reaction system was saturated therewith. Thereafter, the whole was stirred at room temperature overnight. After the completion of the reaction was confirmed, the reaction solution was poured into water and extracted with diethyl ether. The resulting organic layer was washed with water and saline, successively, and then dried over anhydrous magnesium sulfate. The solvent was removed by evaporation under reduced pressure and a gas chromatographic analysis was conducted to confirm that 5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazole-4-carbaldehyde was formed in an amount of 8.8%.

1. stirringThereafter, the whole was stirred at room temperature overnight
2. extractionextracted with diethyl ether
3. washThe resulting organic layer was washed with water and saline
4. dry with materialsuccessively, and then dried over anhydrous magnesium sulfate
5. customThe solvent was removed by evaporation under reduced pressure
6. customwas formed in an amount of 8.8%

ORD record

ord-dc0cb82ca1794c548e6f86764f00ea91

Source dataset

uspto-grants-2007_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07256298B2