HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68453297, compound → HCID 68454248, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68453297 | HCID 68453297 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68454248 | HCID 68454248 | — |
Reaction Steps
HCl (7.2 ml, 4M in dioxane) was added dropwise to a solution of 1,1-dimethylethyl 2-(4-biphenylyl)-N-{[(1,1-dimethylethyl)oxy]carbonyl}alaninate (1.14 g, 2.87 mmol) in CH2Cl2 (10 ml) at 0° C. under argon. The resulting mix was stirred at room temperature for 16 h. The reaction mixture was concentrated leaving a white solid which was refluxed in methanolic HCl (30 mL) for 16 h. The reaction mixture was concentrated and the residue was taken into Na2CO3 (10%, 100 ml) and the product was extracted by EtOAc (3×20 ml). The combined extracts were washed by water then brine, dried and concentrated left 830 mg as a clear oil. MS (ES) m/e 256.2 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07749998B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-363971ce0e0141a7bd9a8f6c75ee21c7 |
| Source note | uspto-grants-2010_07 |