Reaktion #477968

Reaktionsgleichung

chloro-methylsulfanyl-methane

2,4-dichloro-phenol

NaH

→

2,4-dichloro-1-methylsulfanylmethoxy-benzene

Ausbeute 124.2%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITwas continued for 16 hrs at ambient temperature
3. 3
   SonstigeThe reaction was quenched by addition of water (150 mL)
4. 4
   Extraktionextracted with diethyl ether (2×100 mL)
5. 5
   WaschenThe combined organic phases were washed with saturated aq. ammonium chloride (2×100 mL)
6. 6
   Trocknendried (Na2SO4)
7. 7
   Filtrationfiltered
8. 8
   Sonstigeevaporated in vacuo

Vorschrift

To a solution of 2,4-dichloro-phenol (10 g, 61.35 mmol) in dry DMF (100 mL) was added NaH (2.06 g, 85.89 mmol, 60% in mineral oil). The mixture was stirred for 30 min. at room temperature followed by dropwise addition of chloro-methylsulfanyl-methane (5.65 mL, 67.48 mmol) and stirring was continued for 16 hrs at ambient temperature. The reaction was quenched by addition of water (150 mL) and extracted with diethyl ether (2×100 mL). The combined organic phases were washed with saturated aq. ammonium chloride (2×100 mL), dried (Na2SO4), filtered and evaporated in vacuo afforded 17 g crude 2,4-dichloro-1-methylsulfanylmethoxy-benzene which was used without further purification in the next step.

Quelle