HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67618154, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Acrylonitrile | HCID 7855 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 10714321 | HCID 10714321 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67618154 | HCID 67618154 | 58.2% |
Reaction Steps
(-)-(3S,4R)-6-Cyano-3,4-dihydro-4-[(1,6-dihydro-6-oxo-3-pyridazinyl)amino]-2,2-bis(methoxymethyl)-2H-1-benzopyran-3-ol (150 mg, 0.40 mmol) obtained in Example 8 and acrylonitrile (0.055 ml, 0.806 mmol) were dissolved in dimethylformamide (3 ml). Potassium carbonate (111 mg) was added and the mixture was reacted at 50° C. overnight. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (methanol:chloroform=1:30) to give 99 mg of the title compound (58%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05719155 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-a0d21df0056f48d8b3efbc0b9294fab5 |
| Source note | uspto-grants-1998_02 |