반응 #364893

반응 방정식

ammonium chloride

2-phenylimidazole

lithium diisopropylamide

dimethyl sulfate

→

1-methyl-2-phenylimidazole

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   기타resulted in the formation of a white suspension
2. 2
   workup.STIRRINGto stir at room temperature for an additional 30 min during which time the solution
3. 3
   기타the tetrahydrofuran was removed by evaporation under reduced pressure
4. 4
   추출The aqueous phase was extracted with 2×100 mL aliquots of dichloromethane
5. 5
   세척The combined organic extracts were washed with dilute ammonium hydroxide and brine
6. 6
   건조The combined organic extracts were dried over anhydrous sodium sulfate
7. 7
   농축concentrated under reduced pressure

실험 절차

A solution of 40 mL tetrahydrofuran containing 1.0 g of 2-phenylimidazole was cooled to 0° C. and 4 mL of 2M lithium diisopropylamide was added dropwise which resulted in the formation of a white suspension. The mixture was stirred for 10 min at 0° C. and then 0.7 mL of dimethyl sulfate was added The reaction was allowed to stir at room temperature for an additional 30 min during which time the solution became homogeneous. Aqueous ammonium chloride was added and the tetrahydrofuran was removed by evaporation under reduced pressure. The aqueous phase was extracted with 2×100 mL aliquots of dichloromethane. The combined organic extracts were washed with dilute ammonium hydroxide and brine. The combined organic extracts were dried over anhydrous sodium sulfate and concentrated under reduced pressure to yield 1 g of 1-methyl-2-phenylimidazole which was used in the next step without further purification or characterization.

출처