HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68688183, compound → HCID 53665853, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68688183 | HCID 68688183 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 53665853 | HCID 53665853 | 95.4% |
Reaction Steps
To a stirred solution of [benzyl-[2-tert-butoxycarbonylamino-3-(4-trifluoromethyl-phenyl)-propionyl]-amino]-acetic acid ethyl ester (1.5 g, 2.95 mmol) in dry CH2Cl2 (50 mL), 4N HCl in dioxane (25 mL, Aldrich) was added and stirred at room temperature for 2 h and then conc in vacuo. The rxn product was partitioned between CH2Cl2 (100 mL) and saturated NaHCO3 (20 mL). The organic layer was separated, dried over MgSO4 and conc in vacuo to give a clear oil. The oil was diluted in dichloroethane (50 mL) and stirred in 60° C. bath for 2 h to yield 1.02 g (95%) of the product as a off white solid. MS (ESI) 363 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07244843B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-73c0e6fb521540888705c316f3597dad |
| Source note | uspto-grants-2007_07 |