Réaction #2307978

Équation de réaction

hexaethylene glycol

phosgene

hexaethylene glycol monomethyl ether

triethylene glycol

phosgene

toluene

→

methyl hexaethylene glycol chloroformate

Solvants

EtOAc

Conditions de réaction

Traitement

1. 1
   Autreremoved
2. 2
   AutreThe phosgene, EtOAc, and toluene were removed by vacuum distillation

Mode opératoire

Monodispersed activated hexaethylene glycol monomethyl ether was prepared analogously to that of monodispersed triethylene glycol in Example 14 above. A 20% phosgene in toluene solution (35 mL, 6.66 g, 67.4 mmol phosgene) was chilled under a N2 atmosphere in an ice/salt water bath. Monodispersed hexaethylene glycol (1.85 mL, 2.0 g, 6.74 mmol) was dissolved in 5 mL anhydrous EtOAc and added to the phosgene solution via syringe. The reaction mixture was kept stirring in the ice bath for one hour, removed and stirred a further 2.5 hours at room temperature. The phosgene, EtOAc, and toluene were removed by vacuum distillation, leaving monodispersed methyl hexaethylene glycol chloroformate as a clear, oily residue.

Source