Bromine → 6-(Trifluoromethyl)pyridazin-3(2H)-one

温度

100 °C

2.6 g (15.65 mmol) of 6-(trifluoromethyl)-4,5-dihydropyridazin-3(2H)-one were dissolved in 20 ml of glacial acetic acid, and the mixture was heated to 100° C. 0.81 ml (15.65 mmol) of bromine was then slowly added dropwise to the solution, and the mixture was stirred at 100° C. for 4 hours. After cooling of the reaction solution, the solvent was removed under reduced pressure and the residue obtained was purified chromatographically on silica gel (mobile phase dichloromethane/methanol 50:1→20:1). This gave 1.34 g (8.15 mmol, 52% of theory) of the title compound.

1. temperatureAfter cooling of the reaction solution
2. customthe solvent was removed under reduced pressure
3. customthe residue obtained
4. customwas purified chromatographically on silica gel (mobile phase dichloromethane/methanol 50:1→20:1)

ORDレコード

ord-2b40619c3fd7440fb762b3e827ee9f1b

出典データセット

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08987256B2