HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 22452740, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 22452760 | HCID 22452760 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22452740 | HCID 22452740 | 92.8% |
Reaction Steps
A mixture of the compound (8.9 g) obtained in Example 48A, 4N KOH (18 ml) and ethanol (150 ml) was stirred under refluxing conditions for 5 hours. The reaction mixture was poured over water and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4) and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with ethyl acetate-hexane (4:1, v/v) to yield ethyl 2-diethylaminomethyl-4-(4-isopropoxy-3-methoxyphenyl)-5,6,7,8-tetrahydrothieno[2,3-b:5,4-c']dipyridine-3-carboxylate (6.5 g, 88%), which was then recrystallized from ethyl acetate-hexane to yield colorless prismatic crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06046189 |
| Source dataset | uspto-grants-2000_04 |
| ORD ID | ord-c9e38c8572814d138ece233766ae4577 |
| Source note | uspto-grants-2000_04 |