HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitric Acid → HCID 19042736, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 19042739 | HCID 19042739 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 19042736 | HCID 19042736 | 65.5% |
Reaction Steps
90.3 g (0.3 mol) of 1,4-dihydro-2,6-dimethyl-4-phenyl-3,5-bis(carboxymethyl)pyridine were added in portions at from 92° to 98° C. to a solution of 375 g of 98% strength nitric acid in 1580 ml of water in the course of 30 minutes. After a further 30 minutes at 95°-98° C., the mixture was cooled to +5° C. and brought to pH 9 with solid potassium carbonate. The mixture was extracted three times with methylene chloride, the combined extracts were concentrated under reduced pressure and the residue was crystallized at 0° C. using 1:1 diethyl ether/pentane (50 ml). 58.8 g (65.5% of theory) of 2,6-dimethyl-4-phenyl-3,5-bis(carboxymethyl)pyridine were obtained as white crystals of m.p. 137°-138° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05637554 |
| Source dataset | uspto-grants-1997_06 |
| ORD ID | ord-fadb2bc25f13406b9d416e649762f4d2 |
| Source note | uspto-grants-1997_06 |