Reaktion #1334881

Reaktionsgleichung

Methyl iodide

1,1-dibromo-2,2-diphenylcyclopropane

n-butyllithium

hexane

→

title compound

Ausbeute 89.0%

1-bromo-2,2-diphenyl-1-methylcyclopropane

Ausbeute 89.0%

Lösungsmittel

THF

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe resulting mixture was stirred for 30 minutes
2. 2
   Temperaturwarmed to room temperature
3. 3
   Extraktionthe organic layer was extracted with toluene
4. 4
   ExtraktionThe toluene extract
5. 5
   Trocknenwas dried over anhydrous magnesium sulfate
6. 6
   Sonstigethe solvent was removed under reduced pressure
7. 7
   SonstigeThe residue was recrystallized from methanol

Vorschrift

Under a nitrogen atmosphere, 1,1-dibromo-2,2-diphenylcyclopropane(10.6 g, 30.0 mmol) obtained in Example 1-(1) and THF (tetrahydrofuran, 120 ml) were placed in a reaction flask and cooled to −70° C. To the mixture, n-butyllithium in hexane (20 ml, 1.57M, 31.4 mmol) was added gradually, and the mixture was stirred at the same temperature for 30 minutes. Methyl iodide (2.1 ml, 33 mmol) was added to the reaction mixture and the resulting mixture was stirred for 30 minutes and then warmed to room temperature. Then, water was added to the reaction mixture and the organic layer was extracted with toluene. The toluene extract was dried over anhydrous magnesium sulfate and then the solvent was removed under reduced pressure. The residue was recrystallized from methanol to give the title compound (7.28 g, 89%) as white crystal.

Quelle