Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 59867937 | HCID 59867937 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 59867908 | HCID 59867908 | 70.1% |
Reaction Steps
A suspension of 450 mg of the compound obtained in Example 185 and 381 mg of iron in acetic acid (5 ml) was stirred at 80° C. for one hour. Water was added to the solution and the resulting mixture was extracted with EtOAc; the organic layer was washed with a saturated aqueous solution of NaHCO3 and with saturated brine, dried over Na2SO4, then, the drying agent was separated by filtration and the solvent was evaporated under reduced pressure. The obtained residue was purified by column chromatography (silicagel 60N; mobile phase: CHCl3/MeOH=20/1 to 10/1; v/v) to obtain 301 mg of the title compound (amorphous).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08030499B2 |
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| Source dataset | uspto-grants-2011_10 |
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| ORD ID | ord-4b15201a155a4291aa425ff9d99197e9 |
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| Source note | uspto-grants-2011_10 |
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