Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | HCID 59568629 | HCID 59568629 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 59568580 | HCID 59568580 | 33.6% |
Reaction Steps
To tert-butyl [4-({(1S)-1-cyano-2-[4-(2,2-dioxido-1,3-dihydro-2-benzothiophen-5-yl)phenyl]ethyl}carbamoyl)tetrahydro-2H-pyran-4-yl]carbamate (Example 34, step (ii), 300 mg) was added formic acid (2 mL) and the mixture heated to 50° C. for 30 min. The mixture was allowed to cool to room temperature and then methanol (5 mL) was added and the mixture evaporated to give an oil. The crude mixture was purified by preparative HPLC (SunFire column) eluting with methanol/0.1% aqueous trifluoroacetic acid to afford a product which was then purified by chromatography on silica eluting with ethyl acetate to give the titled compound (82 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08193239B2 |
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| Source dataset | uspto-grants-2012_06 |
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| ORD ID | ord-5a0f656f788b487796ce3cd7c84f4610 |
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| Source note | uspto-grants-2012_06 |
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