Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Isocyanate | HCID 105034 | — |
| Reactant | HCID 11374331 | HCID 11374331 | — |
| Product | HCID 10282540 | HCID 10282540 | 90% |
Reaction Steps
The secondary amine (7) obtained in Stage 2 of Example 24 (145 mg, 1 eq, 0.32 mmol) is introduced in solution in dichloromethane (10 mL) into tubes (10). Then the corresponding isocyanate (from 1.09 to 1.17 eq) is added to each tube. The reaction media are stirred for 2 hours at ambient temperature. The PS-Tisamine (reagent supported on resin) (3 eq/excess of isocyanate) is then introduced into each of the tubes, and the reaction media are stirred again for 45 minutes at ambient temperature. This operation is carried out again if any isocyanate remains. The resin is then eliminated by filtration, and the solvent is driven off using a centrifuge under vacuum (speedvac), in order to finally recover the desired product originating from the condensation carried out. In this way the desired urea is obtained with a yield of approximately 90%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07605261B2 |
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| Source dataset | uspto-grants-2009_10 |
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| ORD ID | ord-f0e363ca29d440cb8899d76da7a62c6f |
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| Source note | uspto-grants-2009_10 |
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