HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 67008022, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 86628448 | HCID 86628448 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Product | HCID 67008022 | HCID 67008022 | — |
Reaction Steps
To a 1:1 mixture of N,N-dimethylformamide: methanol saturated with CO, was added the product from Example 9C (5.29 g, 15.6 mmol), palladium (II) acetate (0.088 g, 0.39 mmol), triphenylphosphine (0.31 g, 1.2 mmol) and triethylamine (4.3 ml, 31 mmol). The reaction was stirred overnight at room temperature under a CO atmosphere. The mixture was then partitioned between water and ether and the organic layer was washed with brine then dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified via silica gel chromatography (gradient elution, 0 to 30% diethyl ether-hexanes) to provide the title compound. MS (DCI/NH3) m/e 247 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07998982B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-21327b50f38f43f9aa05977fda542b5e |
| Source note | uspto-grants-2011_08 |