HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 11583653, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86602940 | HCID 86602940 | — |
| Catalyst | HCID 178502593 | HCID 178502593 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 11583653 | HCID 11583653 | 26% |
Reaction Steps
The compound (53 mg, 40.4 mmol) synthesized in Example 14 (14f) was dissolved in methanol (10 mL) and hydrochloric acid (10 μL) and 20% palladium hydroxide-carbon (53 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 (5 mg, 26%) as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07361744B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-d0e8b4422df643d0a34ddcfc4af3bbdf |
| Source note | uspto-grants-2008_04 |