Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 67242533 | HCID 67242533 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57617803 | HCID 57617803 | 100% |
Reaction Steps
To a solution of methyl 2,2-dimethyl-5-(phenylsulfonyl)-2,3,4,5-tetrahydrobenzo[b][1,4]thiazepine-7-carboxylate (450 mg, 1.149 mmol) in THF (10 mL), MeOH (10.00 mL) and water (10.00 mL) was added lithium hydroxide (55.1 mg, 2.299 mmol). The reaction was allowed to stir at room temperature for 8 h. The solvent was removed under reduced pressure. The aqueous solution was acidified with 1 N HCl (10 mL), which resulted in the formation of a white solid. The mixture was washed with EtOAc (3×30 mL) and the combined organics were dried over Na2SO4 and concentrated in vacuo. 2,2-dimethyl-5-(phenylsulfonyl)-2,3,4,5-tetrahydrobenzo[b][1,4]thiazepine-7-carboxylic acid (434 mg, 1.149 mmol, 100% yield) was isolated as an off white solid and used without further purification. LCMS (+ESI) m/z=377.9 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07960376B2 |
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| Source dataset | uspto-grants-2011_06 |
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| ORD ID | ord-9455c7b87dba4402b1f7131930869fb2 |
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| Source note | uspto-grants-2011_06 |
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