HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-t-Butoxycarbonylamino-N-[2,3,4,5-tetrahydro-2-oxo-1-[[2'-[N-(triphenylmethyl)tetrazol-5-yl][1,1'-biphenyl]-4-yl]methyl]-1H-1-benzazepin-3-yl]-butanamide → HCID 178453476, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-t-Butoxycarbonylamino-N-[2,3,4,5-tetrahydro-2-oxo-1-[[2'-[N-(triphenylmethyl)tetrazol-5-yl][1,1'-biphenyl]-4-yl]methyl]-1H-1-benzazepin-3-yl]-butanamide | HCID 19025507 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178453476 | HCID 178453476 | 71% |
Reaction Steps
The intermediate obtained in Step B (349 mg, 0.40 mmol) was dissolved in 5 mL of methanol and hydrogenated at room temperature and one atmosphere over 70 mg of 20% Pd(OH)2 /C for 16 hours. The reaction mixture was filtered through Celite and solvent removed under vacuum. The crude product was purified by flash chromatography on silica, eluting with 10% methanol/ethyl acetate to afford 168 mg (0.28 mmol, 71%) of product. 1H NMR (200 MHz, CD3OD): 1.41 (s,9H), 1.72 (m,2H), 2.0-2.6 (m,6H), 3.24 (t,7 Hz,2H), 4.32 (m,1H), 4.85 (d,14 Hz,1H), 5.20 (d,14 Hz,1H), 6.9-7.7 (m,12H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05206235 |
| Source dataset | uspto-grants-1993_04 |
| ORD ID | ord-4b95ce941ece4cc1adef8de645b56cf4 |
| Source note | uspto-grants-1993_04 |