반응 #932311

반응 방정식

pyridine

1-chloroethyl chloroformate

2-methyl-1-butanol

→

1-chloroethyl 2-methylbutyl carbonate

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture is stirred for 30 minutes
2. 2
   여과The salt precipitate is collected by filtration
3. 3
   세척the filtrate is washed with two 200-ml portions of water
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
6. 6
   workup.DISTILLATIONthe residue is further distilled under reduced pressure

실험 절차

In 70 ml of dichloromethane are dissolved 13 ml of 2-methyl-1-butanol and 17 g of 1-chloroethyl chloroformate, and the solution is cooled to 0° C. With stirring, a solution of 9.6 ml of pyridine in 30 ml of dichloromethane is added dropwise, and the mixture is stirred for 30 minutes. The salt precipitate is collected by filtration and the filtrate is washed with two 200-ml portions of water and dried over anhydrous sodium sulfate. The solvent is then distilled off under reduced pressure and the residue is further distilled under reduced pressure to give 12.5 g of 1-chloroethyl 2-methylbutyl carbonate.

출처