Reaction equation
[CH2:1](O)COCCOCCO.C(Cl)(Cl)=O.C1(C)C=CC=CC=1.[CH2:22]([OH:40])[CH2:23][O:24][CH2:25][CH2:26][O:27][CH2:28][CH2:29][O:30][CH2:31][CH2:32][O:33][CH2:34][CH2:35][O:36][CH2:37][CH2:38][OH:39]>CCOC(C)=O>[CH3:1][O:39][CH2:38][CH2:37][O:36][CH2:35][CH2:34][O:33][CH2:32][CH2:31][O:30][CH2:29][CH2:28][O:27][CH2:26][CH2:25][O:24][CH2:23][CH2:22][OH:40]Participants
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Procedure
The following description refers to the scheme illustrated in FIG. 10. Non-polydispersed activated hexaethylene glycol monomethyl ether was prepared analogously to that of non-polydispersed triethylene glycol in Example 39 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. Non-polydispersed hexaethylene glycol 50 (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 non-polydispersed compound 51 as a clear, oily residue.
Workup
- customremoved
- customThe phosgene, EtOAc, and toluene were removed by vacuum distillation
Sources & evidence
- ORD record
- ord-30eb1584f3b64380bac531cfebd97b41
- Source dataset
- uspto-grants-2006_08
- Patent number
- US07084114B2
Linked notes
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