HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 58166466, compound → HCID 178484255, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 58166466 | HCID 58166466 | — |
| Solvent | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| Product | HCID 178484255 | HCID 178484255 | 85.3% |
Reaction Steps
4-Amino-5-fluoro-1-(thiophen-3-yl)pyrimidin-2(1H)-one (140 mg, 0.66 mmol) was dissolved in DMF-DMA (5 mL). The reaction mixture was stirred at reflux overnight. The residual DMF-DMA was removed in vacuo, and the residue was purified by preparative thin layer chromatography to give (E)-N′-(5-fluoro-2-oxo-1-(thiophen-3-yl)-1,2-dihydropyrimidin-4-yl)-N,N-dimethylformimidamide (75 mg, 43%) as a yellow solid: mp 211-213° C.; 1H NMR (300 MHz, DMSO-d6) δ 8.73 (s, 1H), 8.22 (d, J=6.4 Hz, 1H), 7.75 (dd, J=3.2, 1.4 Hz, 1H), 7.60 (dd, J=5.2, 3.2 Hz, 1H), 7.34 (dd, J=5.2, 1.4 Hz, 1H), 3.26 (s, 3H), 3.13 (s, 2H); ESIMS m/z 267 ([M+H]+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916579B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-e3c16535feb648bbbc55683021a6531c |
| Source note | uspto-grants-2014_12 |