HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 178461967, compound → HCID 178461935, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 178461967 | HCID 178461967 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 178461935 | HCID 178461935 | 93.2% |
Reaction Steps
(S)—N-[4-Fluoro-2-(pyrimidin-4-ylamino)phenyl]-2-(9H-purin-6-ylamino)thiopropionamide (9 mg, 0.02 mmol) was heated in toluene at reflux under nitrogen for 15 h. The reaction mixture was purified by column chromatography (Si—PCC, gradient 0-10% (9:1 MeOH/0.880 NH3) in DCM). Product containing fractions were evaporated and freeze dried to give 332 as a colourless solid, (7 mg, 85%). LCMS (Method C): RT 2.82 min [M+H]+ 376.02 1H NMR (DMSO-d6) δ: 12.8 (1H, bs), 9.20 (1H, s), 8.95 (1H, d, J=5.41 Hz), 8.01-7.89 (4H, m), 7.73 (1H, dd, J=8.81, 4.94 Hz), 7.46 (1H, dd, J=9.30, 2.50 Hz), 7.18 (1H, td, J=9.27, 2.48 Hz), 6.03 (1H, bs), 1.71 (3H, d, J=6.78 Hz)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653089B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-e677a9b353c04ecba0f06d2543d3a3dc |
| Source note | uspto-grants-2014_02 |