HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4-Diaminopyridine → HCID 178488901, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4-Diaminopyridine | HCID 5918 | — |
| Reactant | 2,4-Dimethoxybenzoic acid | HCID 7052 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | HCID 178488901 | HCID 178488901 | — |
Reaction Steps
A mixture of 2,4 dimethoxybenzoic acid (2.5 g) and 3,4-diaminopyridine (1.5 g) was ground to a fine powder and added portionwise to phosphorus oxychloride (50 ml) with stirring. The mixture was stirred and heated under reflux for 2.5 hours before excess phosphorus oxychloride was removed in vacuo. The residue was cooled, water (20 ml) added and the pH adjusted to 7 with ammonium hydroxide to yield a pale yellow solid which was collected, washed with water and dried. The solid was recrystallised twice from aqueous ethanol to yield a cream coloured crystalline solid m.p. 195°-198°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04603139 |
| Source dataset | uspto-grants-1986_07 |
| ORD ID | ord-e9c5bbaa894449bbbd49705cc72ce31f |
| Source note | uspto-grants-1986_07 |