HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 23136406, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Iodine | HCID 807 | — |
| Reactant | Samarium | HCID 23951 | — |
| Reactant | HCID 67145905 | HCID 67145905 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23136406 | HCID 23136406 | 60% |
Reaction Steps
To a mixture of methyl (E)-3-[4-[(2,3-dihydro-1H-inden-1-yl)oxy]-3,5-difluorophenyl]-2-propenoate (0.52 g, 1.6 mmol), samarium (1.2 g, 7.9 mmol), tetrahydrofuran (3 mL) and methanol (7 mL) was added iodine (0.80 g, 3.2 mmol), and the reaction mixture was stirred at room temperature overnight. 1 N Hydrochloric acid (20 mL) was added thereto, and the mixture was stirred for 20 minutes, then diluted with water and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate and concentrated. The residue was purified with silica gel column chromatography (hexane/ethyl acetate=10:1) to give the title compound. Yield 60%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08008525B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-1325dfc932b245cab9133082dd945a66 |
| Source note | uspto-grants-2011_08 |