HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 21083998, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 21084046 | HCID 21084046 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 21083998 | HCID 21083998 | 80% |
Reaction Steps
A mixture of the compound of Example 120 (150 mg, 0.357 mmol) and lithium hydroxide monohydrate (30 mg, 0.714 mmol) in dioxane (3 mL) and water (3 mL) was heated under reflux for 1.5 h. The dioxane was removed in vacuo, the aqueous residue acidified (2M HCl) and the precipitate filtered off and dried to give the title compound as a pale orange solid (112 mg, 80%). δH (DMSO-d6) 13.06 (1H, br s), 8.29 (1H, dd, J 1.3, 8.2 Hz), 8.02–7.93 (2H, m), 7.88–7.84 (1H, m), 7.46–7.35 (6H, m), 6.46 (1H, d, J 9.7 Hz). LCMS (ES+) RT 3.137 minutes, 393.0 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176215B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-634cb3a1348943ea90669a09f59df4fd |
| Source note | uspto-grants-2007_02 |