HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67288468, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 67287501 | HCID 67287501 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67288468 | HCID 67288468 | 36.9% |
Reaction Steps
Methyl 6-cyano-7-(4-(2-(5-(trifluoromethyl)-pyridin-2-yl)ethylcarbamoyl)phenoxy)chroman-4-carboxylate (14.2 mg, 0.0270 mmol) was dissolved in THF (3 mL) and 1M solution of lithium hydroxide monohydrate in water (54.0 μl, 0.0540 mmol) was added. The mixture was stirred overnight at ambient temperature, then quenched with 4.0 M HCl solution in 1,4-dioxane (20.3 μl, 0.0811 mmol). The reaction mixture was purified on silica gel (MeOH in dichloromethane with 1% acetic acid gradient) to provide 5.1 mg of the title compound as a thin film (37%). MS (apci) m/z=509.7 (M−H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785445B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-6f74a0f7e4dd4c029e81e6fc120f2cb6 |
| Source note | uspto-grants-2014_07 |