Reaktion #932311

Reaktionsgleichung

pyridine

1-chloroethyl chloroformate

2-methyl-1-butanol

→

1-chloroethyl 2-methylbutyl carbonate

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture is stirred for 30 minutes
2. 2
   FiltrationThe salt precipitate is collected by filtration
3. 3
   Waschenthe filtrate is washed with two 200-ml portions of water
4. 4
   Trocknendried 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

Vorschrift

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.

Quelle