HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 70941574, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 71059752 | HCID 71059752 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 70941574 | HCID 70941574 | 95.2% |
Reaction Steps
An aqueous solution of 4 mol/L sodium hydroxide (1.55 mL, 6.20 mmol) and water (1 mL) were added to a solution of 2-(4,4-difluoropiperidino)-5-phenyl-7-thiazolo[4,5-b]pyridinecarboxylic acid ethyl ester (500 mg, 1.24 mmol) prepared above in 1,4-dioxane (5 mL), followed by stirring at room temperature for 3 hr. The reaction solution was concentrated, and a saturated aqueous solution of ammonium chloride was added to the residue. The precipitated crystals were collected by filtration, washed with water, and dried. The resulting crude crystals were subjected to recrystallization from acetic acid-water to obtain the title compound (442 mg, 1.18 mmol) as a yellow powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796320B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-677822ca17d640b98fd93c678ffc00cc |
| Source note | uspto-grants-2014_08 |