HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 11496503, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 86602941 | HCID 86602941 | — |
| Catalyst | HCID 178502593 | HCID 178502593 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 11496503 | HCID 11496503 | 73.3% |
Reaction Steps
The compound (115 mg, 86.8 μmol) synthesized in Example 15 (15a) was dissolved in methanol (20 mL) and ethyl acetate (1 mL) and hydrochloric acid (10 μL) and 20% palladium hydroxide-carbon (115 mg) were added thereto, followed by stirring of the mixture at room temperature under a hydrogen atmosphere for 4 hours. After celite filtration, the solvent was distilled off under reduced pressure and the residue was purified by ion exchange resin (Dowex 50w×8) column (water—5% ammonia water). Further, it was purified using silica gel flash column chromatography (ethyl acetate:methanol:water, 1:1:1, V/V) to obtain the desired title compound (30 mg, 73%) as a colorless amorphous.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07361744B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-93cd5b93e3044e2a9173ad78cfa79280 |
| Source note | uspto-grants-2008_04 |