HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 70152942, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 11328099 | HCID 11328099 | — |
| Reactant | HCID 12824445 | HCID 12824445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 70152942 | HCID 70152942 | — |
Reaction Steps
(±)-4-Benzyl-2-[(4-iodo-2-methoxyphenoxy)methyl]morpholine (360 mg, 0.82 mmol), 1-methoxyvin-1-yl trimethyltin (528 mg, 2.4 mmol), and palladium bis(triphenylphosphine)palladium(II)chloride (36 mg, 0.052 mmol) was refluxed in THF (15 ml) for 24 h. Water was added and was followed by extraction twice with ethyl acetate. The solvent was evaporated and the residue was stirred in aqueous hydrochloric acid (25 ml, 1 M) and methanol (10 ml) at 50° C. for 1 h. The product was extracted with ethyl acetate. Drying and evaporation of the solvent was followed by chromatography. The product was dissolved in ether and precipitated as the oxalate. Yield 40 mg. mp 122-127° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06207662B1 |
| Source dataset | uspto-grants-2001_03 |
| ORD ID | ord-0301738c26a54b7db2c409b35f5f6bbc |
| Source note | uspto-grants-2001_03 |