HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 59216441, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 902040 | HCID 902040 | — |
| Reactant | 3-Amino-5-bromo-1-methyl-1,2-dihydropyridin-2-one | HCID 52911268 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59216441 | HCID 59216441 | 26% |
Reaction Steps
To a solution of (6-Chloro-pyridin-3-yl)-(4-methyl-piperazin-1-yl)-methanone (2.00 g, 7.46 mmol) in 10 mL dimethylformamide was added 3-Amino-5-bromo-1-methyl-1H-pyridin-2-one (1.80 g, 8.95 mmol) and sodium hydride (537 mg, 22.4 mmol). After stirring for 18 hours, this was quenched with water. This was extracted with ethylacetate. The ethylacetate layer was dried over anhydrous sodium sulfate, concentrated in vacuo, and purified by flash chromatography (gradient elution 0 to 5% methanol/dichloromethane) to yield 5-Bromo-1-methyl-3-[5-(4-methyl-piperazine-1-carbonyl)-pyridin-2-ylamino]-1H-pyridin-2-one (900 mg, 1.94 mmol). MS (ESI) 406.0 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07683064B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-ca2131b576614b1797b46a615aa70d4e |
| Source note | uspto-grants-2010_03 |