تفاعل #1519090

ord-9d292c769bb142f3b8b5736b119affe3

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىremoved
  2. 2
    أخرىThe phosgene, EtOAc, and toluene were removed by vacuum distillation

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07611864B2uspto-grants-2009_11