HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 117839924, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 117840224 | HCID 117840224 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 117839924 | HCID 117839924 | — |
Reaction Steps
To a methanol solution (1.0 mL) of ethyl 5-(1,1-difluoroethyl)thiophene-2-carboxylate (28.6 mg, 0.130 mmol) synthesized in Reference Synthesis Example 123, 1 M sodium hydroxide aqueous solution (312 μL, 0.312 mmol) was added and the resultant mixture was stirred at room temperature for 1 day. After completion of the reaction, the reaction solution was concentrated under reduced pressure and separated with toluene-water. To the water phase, 12 M hydrochloric acid was added until pH reached 2 and extraction from the resultant mixture with ethyl acetate was performed. The organic layer was concentrated under reduced pressure to obtain a crude product of the title compound. The crude product was used in the next step as it was.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403798B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-863527f101f84ebfb4b90bcf4b338bf6 |
| Source note | uspto-grants-2016_08 |