HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178461160, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 178461164 | HCID 178461164 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178461160 | HCID 178461160 | — |
Reaction Steps
Benzyl (5R,7S)-4-(cyclohexylamino)-1-(3-fluorophenyl)-7-methyl-2-oxo-1,3,8-triazaspiro[4.5]dec-3-ene-8-carboxylate (27.9 g, 0.057 moles) was suspended in MeOH (˜200 mL) and methanolic HCl was added until the solids all went into solution. Pd(OH)2 (4 g, moisture content 60%) was added and the reaction was flushed with hydrogen and kept under a hydrogen balloon. The reaction was stirred at room temperature for 30 min. The reaction was evacuated and recharged with H2 once to remove CO2. The reaction was filtered through celite and concentrated, then the free base was obtained by portioning between CHCL3 and 1 N NaOH. The organic was dried over MgSO4, filtered and evaporated to give the product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08211904B2 |
| Source dataset | uspto-grants-2012_07 |
| ORD ID | ord-62fbc73e4615427082f0281763f9929e |
| Source note | uspto-grants-2012_07 |