HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 14878742, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Acetylpiperazine | HCID 83795 | — |
| Reactant | 2,6-Dichloro-3-nitropyridine | HCID 85239 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 14878742 | HCID 14878742 | 136.1% |
Reaction Steps
A solution of 51.22 g of N-acetylpiperazine in 200 ml of acetonitrile was added over 50 minutes at 0° C. to a mixture of 78 g of 2,6-dichloro-3-nitropyridine, 600 ml of acetonitrile and 66.3 g of potassium carbonate. The mixture was allowed to return to room temperature and was stirred for 75 minutes. The inorganic salts were filtered off and after 180 ml of N,N-diethylamine and 76 g of potassium carbonate were added to the filtrate, the mixture was refluxed for 75 minutes. The inorganic salts were filtered off after cooling and the filtrate was evaporated to dryness under reduced pressure. The 166.9 g of residue were crystallized from 200 ml of ethyl acetate to obtain 87.4 g of the expected product melting at 120° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05081113 |
| Source dataset | uspto-grants-1992_01 |
| ORD ID | ord-184c3f3eb5cf4c42b2c2b41c7117b039 |
| Source note | uspto-grants-1992_01 |