HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 68159059, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Tert-butoxycarbonylalanine | HCID 85082 | — |
| Reactant | HOAt | HCID 181649 | — |
| Reactant | HCID 68156998 | HCID 68156998 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68159059 | HCID 68159059 | 24% |
Reaction Steps
A solution of 4-fluoro-N2-methyl-3-pyridin-2-yl-benzene-1,2-diamine (0.75 g, 3.44 mmol), Boc-Ala (0.72 g, 3.78 mmol), HOAt (0.52 g, 3.78 mmol) in DCM (10 mL) was cooled to 0° C. EDC (0.73 g, 3.78 mmol) was added portion wise and the resulting mixture was stirred for 1 h. The mixture was diluted with DCM (20 mL) and the organic layer was washed with citric acid, brine, dried (MgSO4) and evaporated. The resulting residue was purified by chromatography (Si—PPC, gradient 0-50% EtOAc/cyclohexane) to afford the title compound as a white solid (0.3 g, 24%). LCMS (Method J): RT 2.42 min [M+H]+ 371
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653089B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-6a585128c9114095b3fb2ce61ea1b4fe |
| Source note | uspto-grants-2014_02 |