HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 67538829, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 67538549 | HCID 67538549 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67538829 | HCID 67538829 | 74.9% |
Reaction Steps
Lithium hydroxide monohydrate (0.27 g, 6.45 mmol) in H2O (5 mL) was added to a solution of 4-tert-butoxycarbonylamino-2-(4-chlorophenyl)-2-fluoro-butyric acid ethyl ester (580 mg, 1.61 mmol) in THF (5 mL) and MeOH (5 mL). After being stirred for 12 hours, the mixture was concentrated in vacuo, diluted with H2O, and extracted with DCM (3 times, discarded). The aqueous phase was then acidified to pH 1 and extracted with DCM (2 times). The organic extracts were dried (Na2SO4), filtered, and concentrated in vacuo to give 4-tert-butoxycarbonylamino-2-(4-chlorophenyl)-2-fluoro-butyric acid (400 mg). The material was used in the following step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680114B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-b3d896d564444d3887259803abfb9ee2 |
| Source note | uspto-grants-2014_03 |