반응 #216343

반응 방정식

3-methylbutylamine

triethylamine

phenyl chloroformate

→

phenyl 3-methylbutylcarbamate

수율 83.2%

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.DISTILLATIONAfter distilling off the solvent under reduced pressure, 200 ml of ethyl acetate and 200 ml of water
2. 2
   workup.ADDITIONwere added to the residue
3. 3
   기타The organic layers were separated
4. 4
   추출water layer was extracted with ethyl acetate (100 ml×3)
5. 5
   세척washed with water and saturated sodium chloride solution successively
6. 6
   건조dried over magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off
8. 8
   기타the crystals separated out
9. 9
   여과were collected by filtration
10. 10
    세척washed with petroleum ether

실험 절차

To a solution of 3-methylbutylamine (20 g, 229 mmol) in 840 ml of dichloromethane were added 35.6 ml triethylamine (255 mmol) and 28.8 ml of phenyl chloroformate (230 mmol) at 0° C. The mixture was stirred for three hours at room temperature. After distilling off the solvent under reduced pressure, 200 ml of ethyl acetate and 200 ml of water were added to the residue. The organic layers were separated and water layer was extracted with ethyl acetate (100 ml×3). The organic layers were combined, washed with water and saturated sodium chloride solution successively and dried over magnesium sulfate. The solvent was distilled off and the crystals separated out were collected by filtration, and washed with petroleum ether to give 39.5 g of phenyl 3-methylbutylcarbamate (83%) as colorless crystals.

출처