HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86279168, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 117652988 | HCID 117652988 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86279168 | HCID 86279168 | 97.1% |
Reaction Steps
EXAMPLE 6 Ethyl 4-(4-{(3-chloropyridin-2-yl)[(3R)-piperidin-3-yl]carbamoyl}phenyl)-1-methyl-1H-pyrazole-5-carboxylate hydrochloride salt (7.65 g, 15.2 mmol) was slurried in 50 mL THF followed by the addition of aqueous NaOH (1 mol/L, 50 mL, 50 mmol). Another 23 mL of water was added and the reaction stirred at room temperature for 1.5 h. THF solvent was removed in vacuo, then pH of residual aqueous phase was adjusted to pH 7 with 1 M aqueous HCl, resulting in precipitation of solids. The solids were collected via filtration and after drying afforded the hydrochloride salt of the title compound as an off-white solid (6.49 g, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09227956B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-3e1fffb21d374194b71ec9fb898889e8 |
| Source note | uspto-grants-2016_01 |