Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl isocyanate | HCID 8022 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 178482379 | HCID 178482379 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178465352 | HCID 178465352 | 74.2% |
Reaction Steps
0.25 g (0.5 mmol) trans-(4-{4-[2-(4-amino-cyclohexyl)-ethyl]-piperazin-1-yl}-5,6-dichloro-pyrimidin-2-yl)-methyl-amine trihydrochloride was dissolved in dry dichloromethane (10 ml). Triethylamine (0.28 ml, 2 mmol) was added followed by the addition of ethylisocyanate (0.06 ml, 0.753 mmol), and the reaction mixture was stirred at room temperature for 4 hours. The solvent was removed in vacuo. The residue was triturated with water, and the precipitate was filtered to give the title compound (0.17 g, 72%) MS (EI): 459.2 (MH+). 1H NMR (300 MHz, DMSO-d6 (TMS)+1 drop of cc. DCl, (ppm)): 0.96 t (3H); 0.88-1.13 m (4H); 1.13-1.31 m (1H); 1.54-1.85 m (6H); 2.74 s (3H); 2.98 q (2H); 2.89-3.16 m (4H); 3.19-3.33 m (1H); 3.34-3.58 m (4H); 4.12-4.30 m (2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08802672B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-e1eecc3dca0746f6bf7de1ca42f19e7e |
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| Source note | uspto-grants-2014_08 |
|---|