HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Methoxide → HCID 53241008, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 68322434 | HCID 68322434 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 53241008 | HCID 53241008 | 18.1% |
Reaction Steps
A solution of methyl N-{[(6-{[4-cyano-2-(trifluoromethyl)phenyl]oxy}-3-pyridinyl)amino]carbonyl}-2-methylalaninate (Intermediate 165, 49 mg) in MeOH (10 mL) was heated at reflux for 10 min. Sodium methoxide (4 mg) was added to the hot reaction mixture and it was left refluxing for 2.5 hours. The solvent was evaporated to dryness and the residue obtained was purified by flash-chromatography (companion system, 12 g Si cartridge), with Cyclohexane/EtOAc as eluents from 70/30 to 50/50, to give two batches. The second batch was purified again by mass directed purification (METHOD K), leading to the desired compound which was gathered to the first batch, to afford the title compound as a white solid (8.2 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09216967B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-f15651fb7d8d482bb1afc15f3ebd93f8 |
| Source note | uspto-grants-2015_12 |