HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide dimethyl acetal → HCID 178484259, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| Reactant | HCID 178509007 | HCID 178509007 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178484259 | HCID 178484259 | 92% |
Reaction Steps
To a magnetically stirred solution of 4-amino-5-fluoropyrimidin-2-ol (4.00 g, 31.0 mmol) in DMF (100 mL) was added N,N-dimethylformamide dimethyl acetal (DMF-DMA; 4.00 g, 34.0 mmol). The mixture was stirred at room temperature for 72 h, diluted with Et2O (200 mL), and filtered. The solid product was washed with heptane to give (E)-N′-(5-fluoro-2-oxo-1,2-dihydropyrimidin-4-yl)-N,N-dimethylformimidamide (5.23 g, 92%) as a white solid: mp 240-243° C.; 1H NMR (300 MHz, DMSO-d6) δ 10.7 (br s, 1H), 8.59 (s, 1H), 7.7 (d, J=5.6 Hz, 1H), 3.18 (s, 3H), 3.06 (s, 3H); ESIMS m/z 185 ([M+H]+), m/z 183 ([M−H]−).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916579B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-5f775b86f5c2416e80761ab04a69b5d0 |
| Source note | uspto-grants-2014_12 |