HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → HCID 57761843, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | HCID 57761294 | HCID 57761294 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57761843 | HCID 57761843 | — |
Reaction Steps
Dissolve the crude methanesulfonic acid 3-(3-{2-morpholin-4-yl-6-[4-(3-trifluoromethyl-pyridin-2-yl)-piperazin-1-yl]-pyrimidin-4-yl}-phenyl)-propyl ester obtained above in THF and heat with an excess of dimethylamine in a sealed tube at 55° C. Concentrate under reduced pressure and partition the residue between aqueous NaHCO3 and EtOAc. Dry the organic layer (Na2SO4) and concentrate under reduced pressure. Purify the residue using preparative plate TLC (MeOH/DCM eluent) to afford the title compound. 1H NMR (CDCl3): δ 1.17 (m, 2H), 2.27 (s, 6H), 2.37 (t, 2H), 2.72 (t, 2H), 3.40 (m, 4H), 3.80 (m, 8H), 3.87 (m, 4H), 6.37 (s, 1H), 7.03 (m, 1H), 7.25 (d, 1H, J=7.1 Hz), 7.35 (dd, 1H), 7.79 (m, 2H), 7.89 (d, 1H, J=7.87 Hz), 8.46 (d, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07566712B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-846b9a20f0c848c3bb962442fea16a67 |
| Source note | uspto-grants-2009_07 |