HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 136084607, compound → HCID 136186365, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 136084607 | HCID 136084607 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 136186365 | HCID 136186365 | 50.1% |
Reaction Steps
A mixture of [N,N′-di(tert-butoxycarbonyl)] 2-(benzyloxycarbonylamino)ethoxy-N-methylguanidine (700 mg, 1.5 mmol), as prepared in the preceding step, 10% Pd/C (70 mg) in methanol (20 mL) and chloroform (5 mL) was hydrogenated under hydrogen (balloon) for 1 h. The catalyst was removed by filtration through Celite, the filtrate was concentrated in vacuo. The residue was purified by flash chromatography (95:5 methylene chloride:methanol saturated with ammonia) to give the title compound as a colorless foam (250 mg, 50%). 1H-NMR (300 MHz, CDCl3) δ4.14 (t, J=5.0 Hz, 2H), 3.09 (s, 3H), 3.06 (q, J=5.0 Hz, 2H), 1.50 (s, 9H), 1.46 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06566379B1 |
| Source dataset | uspto-grants-2003_05 |
| ORD ID | ord-1698a8463ffe4e57814984f985c31971 |
| Source note | uspto-grants-2003_05 |