Reaktion #74901

Reaktionsgleichung

2-chloro 1,1,2-trifluoroethylthio nitrobenzene

3-nitrothiophenol

potassium hydroxide

2-chloro-1,1,2-trifluoroethylene

→

3(2-Chloro-1,1,2-trifluoroethylthio) nitrobenzene

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONA mixture of 50 g
2. 2
   TemperaturThe reaction mixture is cooled
3. 3
   Sonstigedecanted
4. 4
   Sonstigethe solution evaporated to dryness in vacuo
5. 5
   workup.ADDITIONis added
6. 6
   Extraktionthe product extracted with methylene chloride
7. 7
   WaschenThe extracts are washed with 2.5 N aqueous sodium hydroxide and water
8. 8
   Sonstigedried
9. 9
   Sonstigeevaporated to dryness in vacuo
10. 10
    Sonstigeaffording 76.5 g

Vorschrift

A mixture of 50 g. (0.322 moles) of 3-nitrothiophenol, 46.6 g. (0.402 moles) of potassium hydroxide, 60 ml. of acetone and 59 g. (0.395 moles) of 2-chloro-1,1,2-trifluoroethylene is heated in an autoclave with stirring for 11/2 hours at 60°-70° C. The reaction mixture is cooled, decanted and the solution evaporated to dryness in vacuo. The oily residue is combined with the solids, water is added and the product extracted with methylene chloride. The extracts are washed with 2.5 N aqueous sodium hydroxide and water, dried and evaporated to dryness in vacuo affording 76.5 g. of 3(2-chloro 1,1,2-trifluoroethylthio nitrobenzene with a b.p. at 0.25 mm. of mercury of 98°-102° C. The structure is verified with nuclear magnetic resonance.

Quelle