Reaktion #4337

Reaktionsgleichung

2-hydroxyethylmethyl sulfide

NaH

1-fluoro-2-nitrobenzene

→

2-(2-methylthioethoxy)-nitrobenzene

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGAfter the suspension has been stirred for 10 hours at 20° C.
2. 2
   workup.DISTILLATIONthe tetrahydrofuran is distilled off in vacuo
3. 3
   workup.ADDITIONWater is added to the residue, and extraction
4. 4
   SonstigeThere is thus obtained an oil which
5. 5
   Sonstigecan be used without further purification for the following hydrogenation stage

Vorschrift

16.3 g of 2-hydroxyethylmethyl sulfide are added dropwise at 20°-25° C. to 8.5 g of a 55% NaH suspension in 150 ml of absolute tetrahydrofuran. The mixture is stirred for 1 hour at 20° C. and for 20 minutes at 40° C., and 25 g of 1-fluoro-2-nitrobenzene are subsequently added at 20° C. After the suspension has been stirred for 10 hours at 20° C., the tetrahydrofuran is distilled off in vacuo. Water is added to the residue, and extraction is repeatedly performed with ether. There is thus obtained an oil which can be used without further purification for the following hydrogenation stage.

Quelle