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 r×n 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 | US07812024B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-03deb643c13a40b3ad68ce6fbd1a7a42 |
| Source note | uspto-grants-2010_10 |