Reaktion #78233

Reaktionsgleichung

2-Fluoro-5-trifluoromethylaniline

potassium O-ethyl dithiocarbonate

sodium nitrite

→

3-ethoxythiocarbonylthio-4-fluorobenzotrifluoride

Ausbeute 99.0%

Lösungsmittel

water

water

water

hydrochloric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   workup.STIRRINGby stirring for 1 hour
3. 3
   ExtraktionThe reaction mixture was extracted with an aqueous solution of ethyl acetate
4. 4
   Sonstigedried
5. 5
   Einengenconcentrated

Vorschrift

2-Fluoro-5-trifluoromethylaniline (14 g) was suspended in 30 ml of water and 10 ml of concentrated hydrochloric acid. The suspension was cooled to −5° C. while a solution of 5.93 g of sodium nitrite in 30 ml of water was added dropwise, followed by stirring at −59° C. for 2 hours. Then the solution was added to a solution of 16 g of potassium O-ethyl dithiocarbonate in 20 ml of water (40 to 50° C.), followed by stirring for 1 hour. The reaction mixture was extracted with an aqueous solution of ethyl acetate, dried and concentrated, giving 22 g of 3-ethoxythiocarbonylthio-4-fluorobenzotrifluoride.

Quelle