Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 10698592 | HCID 10698592 | — |
| Product | HCID 10505011 | HCID 10505011 | 70% |
Reaction Steps
A mixture of the compound obtained in Example 1A (4.02 g) and 3N HCl (12 ml) was stirred at 80° C. for 13.5 hours. After the reaction mixture was alkalinized with 1N NaOH, it was extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried (MgSO4), after which the solvent was distilled off. The residue was subjected to silica gel column chromatography and eluted with chloroform-methanol (30:1, v/v) to yield ethyl 2-(N,N-diethylaminomethyl)-4-(3,4-dimethoxyphenyl)-5,6,7,8-tetrahydrothieno-[2,3-b:5,4-c']dipyridine-3-carboxylate (for structural formula, see below) (2.30 g, 70%) as an amorphous solid having a melting point of 72 to 75° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06046189 |
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| Source dataset | uspto-grants-2000_04 |
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| ORD ID | ord-cb69fcb8d63f4355a872fb495d44680b |
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| Source note | uspto-grants-2000_04 |
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