HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-(3-Nitro-2-pyridinyl)-4-carbobenzoxypiperazine-2-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Chloro-3-nitropyridine | HCID 79613 | — |
| Reactant | 4-((Benzyloxy)carbonyl)piperazine-2-carboxylic acid hydrochloride | HCID 45072677 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | 1-(3-Nitro-2-pyridinyl)-4-carbobenzoxypiperazine-2-carboxylic acid | HCID 23339769 | — |
Reaction Steps
A solution of 6.0 g. of 4-carbobenzoxypiperazine-2-carboxylic acid hydrochloride, 3.3 g. of 2-chloro-3-nitropyridine and 15 ml. of triethyl amine in 100 ml. of dimethyl sulfoxide is heated at 60° with stirring for 18 hours. The mixture is diluted with 400 ml. of water, acidified to pH 3 with concentrated hydrochloric acid, and extracted repeatedly with ether. The combined ether extracts are dried (MgSO4) and concentrated. The residue is crystallized from ethyl acetate/heptane to give 6.3 g. of the title product, m.p. 145°-147°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04138564 |
| Source dataset | uspto-grants-1979_02 |
| ORD ID | ord-db169d516f694ca6b21cdc3424535eec |
| Source note | uspto-grants-1979_02 |