HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 90050662, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 118023175 | HCID 118023175 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 90050662 | HCID 90050662 | — |
Reaction Steps
A mixture of methyl 1,1-difluoro-2′-oxo-1,1′,2′,3-tetrahydrospiro[indene-2,3′-pyrrolo[2,3-b]pyridine]-6-carboxylate (100 mg, 0.30 mmol) and aqueous 6 N sodium hydroxide solution (0.15 mL, 0.91 mmol) in MeOH (5 mL) is heated at reflux for 1 h. The mixture is allowed to cool to ambient temperature before it is acidified to pH ˜6 with aqueous 1 N hydrochloric acid solution. The resulting mixture is filtered, and the filtrate is concentrated. The residue is partitioned between water (10 mL) and 2-methyltetrahydrofuran (2-MeTHF, 10 mL). The aqueous layer is extracted with 2-MeTHF (5×10 mL), and the combined organic layers are dried over sodium sulfate and concentrated in vacuo to provide the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09296750B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-d86cc8804f204b4eb7f111049a5f043f |
| Source note | uspto-grants-2016_03 |