Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Ammonium formate | HCID 2723923 | — |
| Reactant | HCID 59703720 | HCID 59703720 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59703815 | HCID 59703815 | 57.4% |
Reaction Steps
Under a nitrogen atmosphere, to a solution of the compound (1.09 g) obtained in Step 9 and ammonium formate (895 mg) in ethanol (15 ml)-methanol (5 ml) was added 10% palladium carbon (1.0 g). After stirring at 85° C. for 1 hr, the catalyst was filtered off. The filtrate was concentrated under reduced pressure, and the residue was partitioned by adding ethyl acetate and water. The organic layer was washed successively with water and saturated brine, dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:1) to give the title compound (596 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08017612B2 |
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| Source dataset | uspto-grants-2011_09 |
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| ORD ID | ord-4628f08620a7476883ce4815cd663282 |
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| Source note | uspto-grants-2011_09 |
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