반응 #1519090

ord-9d292c769bb142f3b8b5736b119affe3

반응 방정식

OCCOCCOCCOCCOCCOCCO
hexaethylene glycol
O=C(Cl)Cl
phosgene
COCCOCCOCCOCCOCCOCCO
hexaethylene glycol monomethyl ether
OCCOCCOCCO
triethylene glycol
O=C(Cl)Cl
phosgene
Cc1ccccc1
toluene
CC(O)COCCOCCOCCOCCOCCO.O=C(O)Cl
methyl hexaethylene glycol chloroformate

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타removed
  2. 2
    기타The phosgene, EtOAc, and toluene were removed by vacuum distillation

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07611864B2uspto-grants-2009_11