HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-(2-Methyl-5-nitroanilino)-4-(3-pyridyl)pyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 43114742 | HCID 43114742 | — |
| Reactant | HCID 178426708 | HCID 178426708 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | 2-(2-Methyl-5-nitroanilino)-4-(3-pyridyl)pyrimidine | HCID 10686149 | — |
Reaction Steps
Under inert atmosphere, 5 g of sodium salt of the β-oxo-3-pyridinepropanal, with HPLC purity of 99% (A %) and salt content of 25% (residue by calcination), and 8 mL hydrochloric acid in isopropanol in 50 mL toluene is suspended. 3.7 g (2-methyl-5-nitrophenyl)guanidine is added, and the mixture is stirred at room temperature for an hour. The mixture is refluxed for 18 hours, removing the water with a Dean Stark apparatus. Once completed the conversion, the suspension is cooled to 10° C., and the precipitate is filtrated; this is crushed in warm water, yielding, upon filtration and drying, 2.5 g of product with HPLC purity of 96% (A %), identified through GC-MS.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08168787B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-223935cc5710448195d315903f702fc1 |
| Source note | uspto-grants-2012_05 |