Pyridine → HCID 18424482, Verbindung

Temperatur

-20 °C

Into a reactor were introduced 2.00 g (8.69 mmol) of the 1,1-bis(4-fluorophenyl)propene and 25 mL of 1,2-dichloroethane under a nitrogen atmosphere. The contents were cooled to −20° C. A mixture of 1.39 g (8.69 mmol) of bromine and 12 mL of 1,2-dichloroethane was added dropwise thereto over 1 hour, and the resultant mixture was stirred at that temperature for 1 hour and then at room temperature for 16 hours. Subsequently, a solution prepared by mixing 0.703 mL (8.69 mmol) of pyridine with 20 mL of toluene was added dropwise thereto over 15 minutes, and this mixture was stirred at 100° C. for 2 hours and then cooled. Saturated aqueous sodium hydrogen carbonate solution was added to the resultant reaction mixture, which was then extracted with toluene. The resultant organic layer was washed with saturated aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate. Thereafter, the solvent was removed under reduced pressure. The concentrate was recrystallized from ethanol to obtain 1.21 g (45%) of the target compound as white crystals.

1. additionwas added dropwise
2. waitat room temperature for 16 hours
3. customSubsequently, a solution prepared
4. additionwas added dropwise
5. waitover 15 minutes
6. temperaturecooled
7. customreaction mixture, which
8. extractionwas then extracted with toluene
9. washThe resultant organic layer was washed with saturated aqueous sodium chloride solution
10. dry with materialdried with anhydrous magnesium sulfate
11. customThereafter, the solvent was removed under reduced pressure
12. customThe concentrate was recrystallized from ethanol

ORD-Eintrag

ord-7479e3df3c184998a6537d36179ead22

Quelldatensatz

uspto-grants-2002_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06455720B1