HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69710452, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 131724356 | HCID 131724356 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 69710452 | HCID 69710452 | 25.3% |
Reaction Steps
To a solution of the product from Step A (0.13 g, 0.41 mmol) in methanol (20 mL) was added palladium-on-carbon (10%, 0.015 g). This mixture was stirred overnight under an atmosphere of hydrogen (0.4 mL of a 2 N HCl in ethanol was added to protect the ethyl ester). The reaction mixture was filtered and purified by reversed phase HPLC (gradient of acetonitrile in water, 0% to 50% with 0.1% trifluoroacetic acid). The desired fractions were combined, concentrated, treated with 2 N HCl in ethanol (10 mL) and evaporated to a residue which was dried under high vacuum at 78° C. overnight to afford an amorphous solid (0.03 g, 20%): LC/MS (+APCI) m/z 290 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06696476B2 |
| Source dataset | uspto-grants-2004_02 |
| ORD ID | ord-014e9d48f59f48e48862e7aa81d3a1b8 |
| Source note | uspto-grants-2004_02 |