HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 52914286, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 67107596 | HCID 67107596 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 52914286 | HCID 52914286 | 71.7% |
Reaction Steps
A mixture of ethyl 6-(benzenesulphonylmethyl)-3-(isoxazol-3-yl)-2-methoxybenzoate (Intermediate 47, 0.03 g), lithium hydroxide (1M aqueous solution, 0.4 ml) and dioxane (1 ml) was stirred at room temperature overnight then heated at 40° C. for 8 hours. It was left to stand at room temperature overnight then heated at 60° C. for 6 hours. The resultant mixture was acidified by addition of concentrated hydrochloric acid followed by addition of isopropanol (˜0.5 ml). The mixture was purified by preparative HPLC (C18), eluting with a mixture of methanol and water containing 0.1% formic acid with a gradient of 40-98% to give 6-(benzenesulphonylmethyl)-3-(isoxazol-3-yl)-2-methoxybenzoic acid (0.02 g) as a clear glass.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09067905B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-95b4d42cd4564155a4ce642db107b8c7 |
| Source note | uspto-grants-2015_06 |