Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Urea | HCID 1176 | — |
| Reactant | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Jeffamine | HCID 15131492 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 131731081 | HCID 131731081 | — |
Reaction Steps
15.0 g (139.5 mmol) of N,N-dimethylcarbamoyl chloride and 80 mL dioxane were added to a 250 mL two-necked flask with a reflux condenser. Then 13.66 g (135 mmol) triethylamine and 14.88 g (approx. 63 mmol) Jeffamine® D-230 (Huntsman) were added. After the slight exothermic evolution of heat subsided, the mixture was stirred for 3 h at 80° C. and for 1 h at 100° C., where a milky yellowish suspension slowly formed. The suspension obtained in this way was filtered twice through a fluted filter. The solvent was driven off on the rotary evaporator at 60° C. Then the product was purified with stirring for 2 h at 100° C. and 0.3 mbar. Approximately 17.0 g of an orange-red, viscous liquid was obtained, with a calculated “urea equivalent weight” of approx. 191 g/eq.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08608899B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-e59423d8262442928c832c5796439e7a |
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| Source note | uspto-grants-2013_12 |
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