HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → HCID 117775189, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 55043537 | HCID 55043537 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 117775189 | HCID 117775189 | 87% |
Reaction Steps
To a solution of 2-amino-5-bromo-N-(4-fluorobenzyl)nicotinamide (200 mg, 0.62 mmol) and NaOH (50 mg, 1.23 mmol) in 10 mL of EtOH was added HCHO (1 mL, 37% in water) and then the mixture was heated at reflux for 30 minutes. After being concentrated in vacuo, the residue was suspended in water and extracted with EtOAc. The organic phase was washed with brine, dried over sodium sulfate and concentrated in vacuo to give the crude product of 6-bromo-3-(4-fluorobenzyl)-2,3-dihydropyrido[2,3-d]pyrimidin-4(1H)-one (180 mg, yield: 87%) without further purification. 1H-NMR (CDCl3, 400 MHz) δ 8.28˜8.32 (m, 2H), 7.26˜7.31 (m, 2H), 7.02 (t, J=8.4 Hz, 2H), 5.01 (s, 2H), 4.68 (d, J=2.4 Hz, 2H). MS (M+H)+: 336/338.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09364482B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-df22b8145b654407899e1fb3b3afcebf |
| Source note | uspto-grants-2016_06 |