HuagongsheHuagongshe Chemistry Print Report · For research reference only
Beta-Alanine → 3-[(1-Cyano-4-hydroxy-7-phenyl-isoquinoline-3-carbonyl)-amino]-propionic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Beta-Alanine | HCID 239 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | 1-Cyano-4-hydroxy-7-phenyl-isoquinoline-3-carboxylic acid methyl ester | HCID 89812944 | — |
| Solvent | 2-Methoxyethanol | HCID 8019 | — |
| Product | 3-[(1-Cyano-4-hydroxy-7-phenyl-isoquinoline-3-carbonyl)-amino]-propionic acid | HCID 71735782 | 55.3% |
Reaction Steps
A mixture of 1-cyano-4-hydroxy-7-phenyl-isoquinoline-3-carboxylic acid methyl ester (46 mg, 0.15 mmol), β-alanine (674 mg, 7.57 mmol) and NaOMe (327 mg, 6.05 mmol) in 2-methoxyethanol (12 mL) was refluxed for 1.5 h. After the mixture was cooled to r.t., solvent was evaporated. The residue was partitioned between EtOAc (50 mL) and water (50 mL). 1 M HCl was added with vigorous stirring until pH was ˜2. The organic layer was dried over MgSO4 and concentrated. The crude product was purified by column chromatography (0-60% EtOAc/hexanes+2% AcOH) to give 30 mg of the title compound as a pale pink solid. MS: (−) m/z 360.07 (M−1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09409892B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-e85c8151dde24edeb131b8fffc882055 |
| Source note | uspto-grants-2016_08 |