HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 23130560, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Ammonia methanol | HCID 21705897 | — |
| Reactant | HCID 23130410 | HCID 23130410 | — |
| Catalyst | Nickel | HCID 935 | — |
| Product | HCID 23130560 | HCID 23130560 | 61.4% |
Reaction Steps
To a solution of 5-(3-chloro-benzyl)thiophene-2-carbaldehyde described in Preparation Example 44 (1.2 g, 5.08 mmol) in 7N ammonia/methanol (40 mL) was added Raney nickel (2 g), and the solution was stirred at room temperature for 17 hours under hydrogen atmosphere. The reaction solution was filtered through Celite pad, the catalyst was removed, then, this filtrate was evaporated in vacuo, the residue was purified by silica gel column chromatography (ethyl acetate, then ethyl acetate:methanol=5:1), and the title compound (740 mg, 3.12 mmol, 61.4%) was obtained as a brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07932272B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-c9d0f2786ed246058a3d1f434c89c620 |
| Source note | uspto-grants-2011_04 |