HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 59179705, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 59179663 | HCID 59179663 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59179705 | HCID 59179705 | 53% |
Reaction Steps
To a solution of methyl 2-(4-(4-chlorobenzyl)-3-methyl-5-oxo-2,5-dihydro-1H-pyrazol-1-yl)-4-methylthiazole-5-carboxylate (0.22 g, 0.57 mmol) in a mixture of tetrahydrofuran (8 mL) and water (2 mL) was added lithium hydroxide monohydrate (0.12 g, 2.88 mmol). The reaction mixture was heated to reflux for 3 hours. The solvent was removed in vacuo, and the residue was neutralized to pH 4˜5 with 10% hydrochloric acid. The resulting precipitate was collected by filtration and dried to afford the title compound in 53% yield (0.11 g): 1H NMR (300 MHz, DMSO-d6) δ 12.29 (br s, 1H), 7.27 (d, J=8.5 Hz, 2H), 7.21 (d, J=8.5 Hz, 2H), 3.52 (s, 2H), 2.56 (s, 3H), 2.14 (s, 3H); MS (ES+) m/z 364.1 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08258160B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-820061eb2c4e4c7c91d1d1a22947e321 |
| Source note | uspto-grants-2012_09 |