HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 10090332, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | HCID 10024433 | HCID 10024433 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 10090332 | HCID 10090332 | 96.5% |
Reaction Steps
To a solution of 1-(4-{4-[4-(2,4-dimethyl-thiazol-5-yl)-pyrimidin-2-ylamino]-phenyl}-piperazin-1-yl)-ethanone (0.67 g, 1.64 mmol) in EtOH (3 mL) was added 2 M aq HCl (25 mL) in a steady stream. The mixture was heated at reflux for 1 h, cooled, and basified by addition of solid Na2CO3. The product was extracted with EtOAc. The combined organics were washed with brine, dried on Na2SO4, filtered, and evaporated to afford the title compound (580 mg) as a yellow solid. 1H-NMR (CDCl3) TM: 2.62 (s, 3H, CH3), 2.63 (s, 3H, CH3), 2.99 (m, 4H, CH2), 3.06 (m, 4H, CH2), 6.81 (d, 1H, J=5.4 Hz, pyrimidinyl-H), 6.89 (m, 3H, Ph-H, NH), 7.44 (m, 2H, Ph-H), 8.31 (d, 1H, J=5.4 Hz, pyrimidinyl-H). MS (ESI+) m/z 367 (C19H22N6S requires 366.5).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07432260B2 |
| Source dataset | uspto-grants-2008_10 |
| ORD ID | ord-cf26bebfacbf4fa8955d636a535556db |
| Source note | uspto-grants-2008_10 |