HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 70664673, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 70654261 | HCID 70654261 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 70664673 | HCID 70664673 | 52% |
Reaction Steps
To a solution of (S)-methyl 3-(4-ethyl-2-methylpiperazin-1-yl)-2-(4-fluorophenyl)quinoxaline-6-carboxylate (80 mg, crude) in methanol (30 mL) was added sodium hydroxide (31.0 mg, 0.78 mmol) and water (1 mL), and the reaction was stirred overnight at room temperature. The reaction mixture was concentrated in vacuo, dissolved in water (30 mL), and adjusted to pH 5 with HCl (3N) to give the precipitate, which was purified by Prep-HPLC with the following conditions [(Agilent 1200 prep HPLC): Column, SunFire Prep C18, 19*50 mm 5 um; mobile phase, water with 0.05% NH3.H2O and CH3CN (10% CH3CN up to 45% in 10 min); Detector, UV 220 nm] to afford (S)-3-(4-ethyl-2-methylpiperazin-1-yl)-2-(4-fluorophenyl)quinoxaline-6-carboxylic acid (40 mg, 52.0%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08912188B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-56a245d4412446aa8fc47c88420cfb86 |
| Source note | uspto-grants-2014_12 |