HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-(4-Chlorophenylmethylamino)-3-nitro-5-chloropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4-Chlorobenzylamine | HCID 66036 | — |
| Reactant | 2,5-Dichloro-3-nitropyridine | HCID 8063331 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Solvent | 5-Ethyl-2-methylpyridine | HCID 7728 | — |
| Product | 2-(4-Chlorophenylmethylamino)-3-nitro-5-chloropyridine | HCID 11066438 | 87% |
Reaction Steps
A solution of 20.9 g of 4-chlorobenzylamine and 15.7 g of 2,5-dichloro-3-nitropyridine in 250 ml of xylene and 20 ml of 2-methyl-5-ethylpyridine is refluxed for 30 hours. After cooling, water is added to the reaction mixture, the resulting mixture is then extracted with ethyl acetate and the organic phase is washed with a dilute solution of hydrochloric acid and dried over magnesium sulfate. The solvent is evaporated off under vacuum and the residue obtained crystallizes from isopropyl ether to give 21.1 g of 2-(4-chlorophenylmethylamino)-3-nitro-5-chloropyridine in the form of crystals melting at 120° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05128359 |
| Source dataset | uspto-grants-1992_07 |
| ORD ID | ord-84a6714208144e968df5e532ad3dcb22 |
| Source note | uspto-grants-1992_07 |