HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 88656388, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2-Amino-3-methylpyridine | HCID 15347 | — |
| Reactant | Tetramethoxypropane | HCID 66019 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 88656388 | HCID 88656388 | — |
Reaction Steps
A solution of 2-amino-3-methylpyridine (53.9 g) and anhydrous hydrogen chloride (40 g) in anhydrous ethanol (960 ml) was treated with 1,1,3,3-tetramethoxypropane and heated at reflux for 6 hours. The solution was then concentrated to dryness under reduced pressure and the residue was triturated with diethyl ether, to give crude 9-methylpyrido[1,2-a]pyrimidinium chloride (76 g). This crude salt was dissolved in water (300 ml) and treated with sodium bicarbonate (35.4 g). The mixture was stirred at room temperature for one hour and then it was filtered, washed with water and recrystallised from water, to give 1-formyl-2-(3-methylpyrid-2-ylamino)ethene (32.7 g), m.p. 129°-131° C. (with decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04659727 |
| Source dataset | uspto-grants-1987_04 |
| ORD ID | ord-a37604ae97ba42cd8dd267c0471b5172 |
| Source note | uspto-grants-1987_04 |