HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 178466934, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Benzamidine, hydrochloride | HCID 80289 | — |
| Reactant | 2-(4-Hydroxy-3-nitrobenzylidene)acetylacetone | HCID 57030162 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 178466934 | HCID 178466934 | — |
Reaction Steps
A mixture of 2-(4-hydroxy-3-nitrobenzylidene)acetylacetone (40 g), benzamidine hydrochloride (30.2 g) and triethylamine (31.2 ml) in n-butanol (400 ml) was refluxed for 2 hours. The reaction mixture, added ethyl acetate (100 ml), was washed with water (200 ml) and 5% hydrochloric acid (200 ml) successively. The solvent was evaporated and the residue was stirred with ethyl acetate (200 ml) for 1 hour. The crystals were collected by filtration, added a mixture of chloroform (200 ml) and water (200 ml) and adjusted to pH 8.5 by saturated potassium carbonate. The organic layer was evaporated in vacuo to give crude 5-acetyl-1,6-dihydro-6-(4-hydroxy-3-nitrophenyl)-4-methyl-2-phenylpyrmidine (45.5 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04698340 |
| Source dataset | uspto-grants-1987_10 |
| ORD ID | ord-fc6db7eb11c4472c8e926d4e8c83ff7a |
| Source note | uspto-grants-1987_10 |