HCID 13058056, compound → 1,2-Dichloro-1-fluoro-2-(trifluoromethoxy)ethene

Temperature

-75 °C

In a 1 l three necked flask, equipped with magnetic stirrer, thermometer, dropping funnel, and connected through a Vigreux column and a condenser to a trap maintained at -75° C., 80.0 g of zinc powder, activated by washing with HCl 3N, 550 ml of DMF and 50 mg of KI were charged under nitrogen atmosphere. The internal temperature was brought to 80° C. and 102.0 g of 1,1,2,2-tetrachloro-1-fluoro-2-trifluoromethoxyethane (377m moles), were added dropwise. During the addition, the temperature increased up to 90° C. When the addition was over, the reaction mixture was stirred for 1 additional hour at 90° C. In the cold trap 62.8 g (315 mmoles) of 1,2-dichloro-1-fluoro-2-trifluoromethoxyethane (cis/trans 50%/50%) condensed. The 1,2-dichloro-1-fluoro-2-trifluoromethoxyethene (trans+cis) yield was 83%.

1. customconnected through a Vigreux column and a condenser to a trap
2. washby washing with HCl 3N, 550 ml of DMF and 50 mg of KI
3. additionwere charged under nitrogen atmosphere
4. customwas brought to 80° C.
5. addition102.0 g of 1,1,2,2-tetrachloro-1-fluoro-2-trifluoromethoxyethane (377m moles), were added dropwise
6. additionDuring the addition
7. temperaturethe temperature increased up to 90° C
8. additionWhen the addition

ORD record

ord-2a301c6b0eca49f0af5036863ec686cf

Source dataset

uspto-grants-1997_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05646223