Phosphorus oxychloride → 2-(1-Methyl-1H-pyrazol-5-yl)-5-[4-(trifluoromethyl)phenyl]-1,3,4-oxadiazole

温度

90 °C

Phosphorus oxychloride (1.80 mL) was added to an acetonitrile (4.8 mL) suspension of 1-methyl-N′-[4-(trifluoromethyl)benzoyl]-1H-pyrazol-5-carbohydrazide (300 mg) at a room temperature, and the obtained solution was then heated to reflux at 90° C. for 15 hours. Thereafter, the reaction solution was concentrated under a reduced pressure. A saturated sodium carbonate aqueous solution was added to the residue to convert it to a basic solution, and the resulting solution was then extracted with ethyl acetate. The organic layer was washed with a saturated saline, and was then dried over anhydrous magnesium sulfate, followed by vacuum concentration, so as to obtain the title compound (230 mg) in the form of a brown solid.

1. temperaturethe obtained solution was then heated
2. concentrationThereafter, the reaction solution was concentrated under a reduced pressure
3. additionA saturated sodium carbonate aqueous solution was added to the residue
4. extractionthe resulting solution was then extracted with ethyl acetate
5. washThe organic layer was washed with a saturated saline
6. dry with materialwas then dried over anhydrous magnesium sulfate
7. concentrationfollowed by vacuum concentration

ORDレコード

ord-666a2e489bbf45ba8bb39f1ebde6a3a4

出典データセット

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08642626B2