HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-(4-Methylpyridin-2-yl)-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | 2-Hydrazinyl-4-methylpyridine | HCID 12266739 | — |
| Reactant | 3-Hydroxy-2-pyridin-3-yl-acrylic acid ethyl ester | HCID 68708088 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 2-(4-Methylpyridin-2-yl)-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one | HCID 59186954 | — |
Reaction Steps
1.53 g (7.90 mmol) of the compound from Example 2A and 2.92 g (23.7 mmol) of the compound from Example 1A are dissolved 2 ml anhydrous ethanol under argon and the mixture is stirred at RT for 16 h. 537 g (7.90 mmol) sodium ethanolate are added, the reaction solution becoming dark red in color. The mixture is subsequently stirred at RT for 30 min and 7.9 ml 1 M hydrochloric acid are then added. The solution is partly concentrated, a precipitate separating out. This is filtered off, washed with water (twice with 5 ml each time) and with MTBE (5 ml) and dried in vacuo. 435 mg (22% of th.) of the title compound are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08252817B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-63bf55f4b9034805bcbdb450d41003c6 |
| Source note | uspto-grants-2012_08 |