HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 12387600, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | Ethyl 4,6-dichloro-2-methyl-5-nitropyridine-3-carboxylate | HCID 12387594 | — |
| Product | HCID 12387600 | HCID 12387600 | — |
Reaction Steps
55.8 g. of 4,6-dichloro-2-methyl-5-nitropyridine-3-carboxylic acid ethyl ester (0.2 mol.) are dissolved in 300 ml. of alcohol. After addition of 25 g. of triethylamine (0.25 mol.), the mixture is heated at reflux temperature and then 20 g. of N-methylpiperazine are dropped in with stirring. When the addition is completed, the temperature is maintained for 30 minutes. The solvent is distilled off, the residue is dissolved in benzene and the precipitated triethylammonium chloride filtered off. After evaporation of the solvent, the residual 4-chloro-2-methyl-6-(4-methyl-1-piperazinyl)-5-nitropyridine-3-carboxylic acid ethyl ester is recrystallized from methanol, yield 40 g. (60%), m.p. 59°-61°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04022779 |
| Source dataset | uspto-grants-1977_05 |
| ORD ID | ord-d226eb7dcf2e41739a3aa9536a64a71f |
| Source note | uspto-grants-1977_05 |