HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 68956958, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 68957633 | HCID 68957633 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68956958 | HCID 68956958 | — |
Reaction Steps
1 M LiOH (34 ml) was added to a solution of 2-cyano-5-[(S)-3-(4-cyano-3-fluorophenoxy)-2-hydroxy-2-methylpropionylamino]benzoic acid methyl ester (4.52 g, 11.4 mmol) in THF (50 ml) and methanol (6 ml) at 16-18° C. The resulting solution was stirred at room temperature for 2.5 h. The solvents were evaporated and pH was adjusted to 2 with HCl solution. The product was extracted into ethyl acetate. The organic phase was washed with water, dried over Na2SO4 and evaporated. The residue was purified by flash chromatography (eluent: CH2Cl2/MeOH 98:2). Trituration in hot CH2Cl2, cooling to room temperature and filtration yielded the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08501814B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-6698e76b11644626aedb4815b547c347 |
| Source note | uspto-grants-2013_08 |