Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 66817001 | HCID 66817001 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 66818171 | HCID 66818171 | 100.1% |
Reaction Steps
LiOH.H2O (16.6 mg, 0.396 mmol) was added to a solution of 1-[(E)-2-(2,6-dimethyl-4-methylamino-phenyl)-ethenesulfonyl]-4-[9-(3-methyl-oxetan-3-yl)-nonanoylamino]-piperidine-4-carboxylic amide (96 mg, 0.098 mmol) in ethanol (1.0 mL), and the mixture was stirred at 50° C. for two hours. A 50% saturated aqueous ammonium chloride solution was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was then dried over MgSO4 and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate) to give 8-[(E)-2-(2,6-Dimethyl-4-methylamino-phenyl)-ethenesulfonyl]-2-[8-(3-methyl-oxetan-3-yl)-octyl]-1,3,8-triaza-spiro[4.5]dec-1-en-4-one (54.8 mg, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09169254B2 |
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| Source dataset | uspto-grants-2015_10 |
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| ORD ID | ord-6690fa9249964eb0a907cc9ff80c86aa |
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| Source note | uspto-grants-2015_10 |
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