HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → Ethyl 5-bromo-2-(4-methyl-1-piperazinyl)-4-pyridinecarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Ethyl 2-(4-methylpiperazin-1-yl)pyridine-4-carboxylate | HCID 2762483 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ethyl 5-bromo-2-(4-methyl-1-piperazinyl)-4-pyridinecarboxylate | HCID 11221145 | 37.4% |
Reaction Steps
A solution of 0.91 ml (17.7 mmol) Br2 was added dropwise to a solution of 2.95 g (11.8 mmol) 2-(4-methyl-piperazin-1-yl)-isonicotinic acid ethyl ester in 20 ml dichloromethane at 0° C.-4° C. Stirring was continued at room temperature for 1 h and 50 ml saturated sodium bicarbonate solution in water was added. The aqueous layer was separated and washed twice with dichloromethane. The combined organic layers were dried (magnesium sulfate) and evaporated. The residue was purified by chromatography to give 1.45 g (37%) of the title compound as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06225316B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-51a2f18772b347b69b9a0b86eefab0f4 |
| Source note | uspto-grants-2001_05 |