HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 18651488, compound → HCID 178453551, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 18651488 | HCID 18651488 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178453551 | HCID 178453551 | 61.1% |
Reaction Steps
The intermediate obtained in Step B (150 mg, 0.18 mmol) dissolved in 5 mL methanol was hydrogenated over 30 mg of Pd(OH)2 on carbon at one atmosphere for 2 hours. The mixture was filtered through Celite and the filtrate concentrated under vacuum. The residue was purified by medium pressure liquid chromatography on silica, eluting with ethyl acetate/acetonitrile/methanol (9:1:1) to afford 62 mg (0.11 mmol, 59%) of the product as a colorless glass. 1H NMR (200 MHz, CD3OD): 1.39 (s,9H), 2.0-2.5 (m,6H), 3.26 (t,7 Hz,2H), 4.31 (dd;7,12 Hz;1H), 4.83 (d,16 Hz,1H), 5.20 (d,16 Hz,1H), 6.98 (d,8 Hz,2H), 7.1-7.6 (m,10H). FAB-MS: calc. for C32H35N7O4 581; found 582 (M+H,19%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05206235 |
| Source dataset | uspto-grants-1993_04 |
| ORD ID | ord-4d3815ed9c224615a37201231cb9efd7 |
| Source note | uspto-grants-1993_04 |