Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Hexane | HCID 8058 | — |
| Reactant | HCID 24707938 | HCID 24707938 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 84071213 | HCID 84071213 | 57% |
Reaction Steps
A solution (1 mL) of the compound (560 mg, 2.28 mmol) of Step 1 in N-methyl-2-pyrrolidinone was irradiated with a microwave in a tightly-sealed container, and stirred at 200° C. for 1 hour. To the reaction solution, ethyl acetate and hexane were added. After washing with water and saturated brine, the resultant was dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure. The residue was purified by silica gel chromatography. To the resulting compound (368 mg, 1.50 mmol), formic acid (2 mL) and water (0.2 mL) were added, and stirred at 100° C. overnight. The reaction solution was diluted with ethyl acetate, and after washed with water and saturated brine, the resultant was dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure. The resulting residue was purified by silica gel chromatography (hexane/ethyl acetate) to thus obtain the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09290487B2 |
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| Source dataset | uspto-grants-2016_03 |
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| ORD ID | ord-2a06de5216474f36bcc9cd889862244d |
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| Source note | uspto-grants-2016_03 |
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