HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86726411, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86726412 | HCID 86726412 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86726411 | HCID 86726411 | 87.5% |
Reaction Steps
4M HCl in Dioxane (0.2 mL) was added directly to the product from step 2 (14 mg, 0.016 mmol) and the reaction stirred at RT for 1 hour. The solvent was removed in vacuo and the residue was dissolved in MeOH and loaded onto a 400 mg Porapak cartridge (preconditioned with 5 mL of MeOH). The cartridge was washed with 100 mL of MeOH, then the desired product was eluted with 10 mL of 2M NH3 in MeOH. The solvent was removed in vacuo to afford 4-fluoro-β-(4-fluorophenyl)-N-(5-fluoro-4-{2-[(2R,5S)-5-({[(2,2,2-trifluoroethyl)carbamoyl]oxy}methyl)morpholin-2-yl]ethyl}pyridin-3-yl)-Nα-[(2-methylpropoxy)carbonyl]-L-phenylalaninamide (10 mg, 0.014 mmol) as a tan solid, LC MS: RT=1.94 min, M+H=740.4 (4 min gradient).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09315475B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-25c831a2aa7e40f4a4e56fb5f392e236 |
| Source note | uspto-grants-2016_04 |