HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 14397387, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | 5-((6-Methyl-3-pyridyl)methyl)-2-(nitroamino)-1H-pyrimidin-4-one | HCID 3018360 | — |
| Reactant | N1-(3,5-Dimethyl-2-pyridinyl)-1,3-propanediamine | HCID 14397363 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 14397387 | HCID 14397387 | — |
Reaction Steps
2-(3-Aminopropylamino)-3,5-dimethylpyridine (0.81 g) and 2-nitroamino-5-(6-methylpyrid-3-ylmethyl)-4-pyrimidone (1.04 g) were fused together on an oil bath at 140° C. for 6 hr. On cooling the resulting mixture was equilibrated between chloroform and water (pH adjusted to 5.5 with dil. hydrochloric acid). The pH of the aqueous solution was raised to 6.5 and the product extracted out with chloroform. After drying (MgSO4) and stripping, recrystallisation from ethyl acetate and finally twice from ethanol/water gave 2-[3-(3,5-dimethylpyrid-2-ylamino)propylamino]-5-(6-methylpyrid-3-ylmethyl)-4-pyrimidone 2.4H2O, (0.83 g; 49%) m.p. 104°-5° C. (softens ca 90° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04652650 |
| Source dataset | uspto-grants-1987_03 |
| ORD ID | ord-1e22c00561f84f73915c73c40f2971fc |
| Source note | uspto-grants-1987_03 |