Reaktion #417310

Reaktionsgleichung

hydrochloric acid

cyclobutylcarbonyl chloride

t-butylmagnesium chloride

→

t-butylcyclobutylketone

Lösungsmittel

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONTo a mixture of 118.5 g
2. 2
   workup.ADDITIONThe addition
3. 3
   Sonstigeis carried out at -5° to -15° C
4. 4
   workup.ADDITIONThe resulting mixture is poured into 500 ml
5. 5
   Sonstigeice, the organic layer is separated
6. 6
   Waschenwashed successively with water, sodium bicarbonate solution, brine
7. 7
   Trocknendried (MgSO4)
8. 8
   ExtraktionThe dried ether extract
9. 9
   Sonstigeis evaporated at reduced pressure
10. 10
    workup.DISTILLATIONthe residue distilled

Vorschrift

To a mixture of 118.5 g. (1.0 mole) of cyclobutylcarbonyl chloride and 99 g. (1.0 mole) cuprous chloride in 1000 ml. of dry ether under a nitrogen atmosphere is added dropwise 478 ml. (1.0 mole) of 2M t-butylmagnesium chloride in the same solvent. The addition is carried out at -5° to -15° C. The resulting mixture is poured into 500 ml. of 3M hydrochloric acid and 700 g. ice, the organic layer is separated and washed successively with water, sodium bicarbonate solution, brine and dried (MgSO4). The dried ether extract is evaporated at reduced pressure and the residue distilled to provide t-butylcyclobutylketone.

Quelle