HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenylphosphonic dichloride → 2-Chloro-3,4-diethoxycarbonyl-6-methyl-5-nitropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenylphosphonic dichloride | HCID 69990 | — |
| Reactant | 3,4-Diethoxycarbonyl-6-methyl-5-nitro-2-pyridone | HCID 19935590 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2-Chloro-3,4-diethoxycarbonyl-6-methyl-5-nitropyridine | HCID 19935584 | — |
Reaction Conditions
| Temperature | 170 °C |
|---|
Reaction Steps
To 1.0 g of 3,4-diethoxycarbonyl-6-methyl-5-nitro-2-pyridone was added 1.3 ml (3.2 eq.) of phenylphosphonic dichloride. The mixture was heated at 170° C. for 20 mintues. Water was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After the solvent was distilled off, the residue was purified by silica gel column chromatography (eluent:ethyl acetate) to give an oily product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05420275 |
| Source dataset | uspto-grants-1995_05 |
| ORD ID | ord-1ee93671a1c449ee91ceaa24da712e78 |
| Source note | uspto-grants-1995_05 |