Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 11031413 | HCID 11031413 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 70250426 | HCID 70250426 | 94% |
Reaction Steps
Compound 6a (31.7 g), iron powder (41.1 g), ammonium chloride (18.1 g), and water (173 ml) were added to a mixed solution of tetrahydrofuran (280 ml) and methanol (280 ml) in a nitrogen atmosphere. The mixture was stirred at 70° C. for 1 hour. After the reaction mixture was allowed to cool, and filtered, the filtrate was separated with ethyl acetate and water. The organic layer was washed once with water and once with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate. The solvent was distilled off, and as a result, Compound 6b (25.7 g, 94%) was obtained as an orange solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07855300B2 |
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| Source dataset | uspto-grants-2010_12 |
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| ORD ID | ord-4c592b0d722c4a6a805b4192174c21a1 |
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| Source note | uspto-grants-2010_12 |
|---|