HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 15007585, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 15007582 | HCID 15007582 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15007585 | HCID 15007585 | — |
Reaction Steps
To a suspension of 6-cyano-3,4-dihydro-2,2-dimethyl-trans-3-hydroxy-4-(4-ethoxy-2-oxo-3-pyrrolin-1-yl)-2H-1-benzopyran (0.5 g) in 25 ml of methylene chloride at 0° C. was added pyridine (0.415 g) and acetic anhydride (0.56 g), and the mixture stirred at room temperature for 5 days. The reaction mixture was then stirred with a mixture of 50 ml of water and 40 ml of methylene chloride. The organic layer was separated, washed with water, dried over anhydrous sodium sulfate and solvent removed under reduced pressure. The residue was triturated with ether followed by pentane to give 6-cyano-3,4-dihydro-2,2-dimethyl-trans-3-acetyloxy-4-(4-ethoxy-2-oxo-3-pyrrolin-1-yl)-2H-1-benzopyran, m.p. 156° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04997846 |
| Source dataset | uspto-grants-1991_03 |
| ORD ID | ord-52d0ecf3fad3410094c94548d16fc216 |
| Source note | uspto-grants-1991_03 |