HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 70970325, compound → HCID 66686477, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 70970325 | HCID 70970325 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66686477 | HCID 66686477 | 58.1% |
Reaction Steps
To a solution of (1S)-1-methyl-2-(2,3,5-trifluorophenyl)ethyl azide (930 mg, 4.32 mmol) in 100 mL of EtOAc was added Pd/C (300 mg of 10% Pd) and the mixture was hydrogenated under hydrogen balloon for 1 h. The catalyst was removed by filtration through celite, then passed through silica gel plug eluting first with EtOAc (40 mL), then MeOH/EtOAc/NH4OH 20:75:5 (120 mL). The fraction with product was evaporated to give (1S)-1-methyl-2-(2,3,5-trifluorophenyl)ethylamine (475 mg, 58%) as pale yellow oil. ESI-MS: m/z (MH+) 190.1. 1H NMR (300 MHz, CDCl3): δ 7.04 (m, 1H), 6.83 (m, 1H), 4.06 (s, 2H), 3.42 (m, 1H), 2.92 (m, 2H), 1.29 (d, J=6.21 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08815906B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-8c6dbfd6321a4797bbe920604659980e |
| Source note | uspto-grants-2014_08 |