HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 59787347, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 59787364 | HCID 59787364 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59787347 | HCID 59787347 | 10% |
Reaction Steps
Add a solution of 3-tert-butoxycarbonyl-7-chloro-6-(thiazol-2-ylethynyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (160 mg, 0.41 mmol) in ethanol (10 mL) to a suspension of 10% Pd/C (Degussa type E101, 160 mg), then acetic acid (0.5 mL). Hydrogenate for 7 h (68-70 psi) then filter the catalyst through Celite® and concentrate in vacuo. Purify by chromatography on silica gel eluting with isohexane/EtOAc (1:0 to 4:1 gradient over 40 min) to obtain the desired intermediate (16 mg, 10%). MS (ES+) m/z: 393 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08420631B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-817f0385d304471cac05ddbf434e2c18 |
| Source note | uspto-grants-2013_04 |