HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 11581279, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 68863340 | HCID 68863340 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 11581279 | HCID 11581279 | 97.2% |
Reaction Steps
A solution of Example 418B (2.0873 g, 5.35 mmol) in 4:1 methanol:ethyl acetate (120 mL) was treated with Raney nickel (4.00 g), pressurized to 60 psi with H2 and shaken for 2 hours. The reaction was then filtered and the filtrate was concentrated to yield the desired product (1.8750 g, 97%). MS (ESI(+)) m/e 361 (M+H)+, 383 (M+Na)+; MS (ESI(−)) m/e 359 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 7.32 (dd, 1H), 7.23 (td, 1H), 7.02 (d, 1H), 6.80 (m, 2H), 6.52 (td, 1H), 3.74 (s, 3H), 2.65 (m, 2H), 2.53 (m, 2H), 1.65 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07491718B2 |
| Source dataset | uspto-grants-2009_02 |
| ORD ID | ord-5bb9b752d3554213952a53b9f0b2fcec |
| Source note | uspto-grants-2009_02 |