HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 66643727, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 66643620 | HCID 66643620 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66643727 | HCID 66643727 | 58% |
Reaction Steps
To a solution of 2-{2-[3-(5-fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-yl]-ethyl}-thiazole-5-carboxylic acid methyl ester (1.27 g, 3.66 mmol) in THF (9 mL) was added a solution of lithium hydroxide monohydrate (307 mg, 7.31 mmol) in water (9 mL) and the resulting mixture stirred at room temperature for 2 h. The mixture was then evaporated to half volume and then acidified to pH 1 with HCl (1 N) and cooled to 0° C. for 15 min. A solid precipitated and was filtered off and dried to afford the title compound (707 mg, 58%) which was obtained as an off white solid after recrystallization from ethyl acetate. MS: m/e=332.3 [M−H]−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08178522B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-f8becba9a545439bae63fb9ff25cbb0c |
| Source note | uspto-grants-2012_05 |