Reaktion #415524

Reaktionsgleichung

3-hexanol

phosgene

→

3-Hexyl chloroformate

Lösungsmittel

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooling in an ice bath
2. 2
   workup.ADDITIONThe addition
3. 3
   workup.WAITGaseous nitrogen is passed through the solution for several hours
4. 4
   Sonstigeto remove the excess phosgene and hydrogen chloride
5. 5
   SonstigeThe reaction mixture is then evaporated to dryness in vacuo
6. 6
   Sonstigeaffording 28.3 g

Vorschrift

20.4 G. (0.2 moles) of 3-hexanol is added dropwise under anhydrous conditions to 345 ml. (0.4 moles) of 12.5% phosgene in benzene with stirring and cooling in an ice bath. The addition is complete in 2 hours and 15 minutes and the temperature is allowed to warm to room temperature and the reaction mixture is stirred overnight. Gaseous nitrogen is passed through the solution for several hours to remove the excess phosgene and hydrogen chloride. The reaction mixture is then evaporated to dryness in vacuo affording 28.3 g. (86%) of a colorless oil which infrared analysis indicates to have a strong carbonyl band and no hydroxy band. The oil is used as is in subsequent reactions.

Quelle