Reaktion #722302

Reaktionsgleichung

carbon disulfide

4-(trans-4-propylcyclohexyl)phenyl bromide

magnesium

hydrochloric acid

→

4-(trans-4-propylcyclohexy)phenyl dithiocarboxylic acid

Ausbeute 17.7%

Lösungsmittel

THF

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a solution obtained
2. 2
   workup.STIRRINGstirred
3. 3
   Temperaturwith reflux for 30 minutes
4. 4
   workup.STIRRINGstirred for one night
5. 5
   Sonstigethe reaction
6. 6
   Extraktionextracted with ether
7. 7
   Trocknendried with anhydrous magnesium sulfate
8. 8
   FiltrationAfter filtering off magnesium sulfate
9. 9
   Einengenthe filtrate was concentrated under reduced pressure

Vorschrift

To a solution obtained by suspending 2.25 g (93 mmol) of magnesium in 50 mL of THF, a solution of 20.0 g (71 mmol) of 4-(trans-4-propylcyclohexyl)phenyl bromide in 100 mL of THF was added dropwise with stirring at the room temperature for 45 minutes and stirred with reflux for 30 minutes, to prepare a Grignard reagent. To the solution, 16.3 g (214 mmol) of carbon disulfide was added dropwise for 15 minutes at the room temperature and stirred for one night. To the reaction solution, 60 mL of 3M hydrochloric acid was added to stop the reaction, extracted with ether, and dried with anhydrous magnesium sulfate. After filtering off magnesium sulfate, the filtrate was concentrated under reduced pressure, to obtain 3.5 g (yield 17.7%) of 4-(trans-4-propylcyclohexy)phenyl dithiocarboxylic acid.

Quelle