HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 14397375, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 6-Chloro-3-pyridinecarbonitrile | HCID 5152094 | — |
| Reactant | HCID 14397373 | HCID 14397373 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 14397375 | HCID 14397375 | — |
Reaction Steps
2-Chloro-5-cyanopyridine (0.61 g), 2-(3-aminopropylamino)-5-(6-methylpyrid-3-ylmethyl)-4-pyrimidone (1.09) and potassium carbonate (0.61 g) were heated together under reflux in pyridine (10 ml) for 2.5 hr. The mixture was stripped, the residue taken up in water and the pH adjusted to 3 with hydrochloric acid. After extracting with chloroform the aqueous solution was filtered and the pH raised to 6.5 with sodium hydroxide. The precipitate thus obtained was chromatographed (silica gel, chloroform/methanol, graded 1:0 to 20:1) and the required component recrystallised twice from ethanol to give 2-[3-(5-cyanopyrid-2-ylamino)propylamino]-5-(6-methylpyrid-3-ylmethyl)-4-pyrimidone 0.2 H2O, (0.38 g; 25%) m.p. 175°-177° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04652650 |
| Source dataset | uspto-grants-1987_03 |
| ORD ID | ord-e25ccb4f187a4fb3bc13709f0220d7f8 |
| Source note | uspto-grants-1987_03 |