Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Dimethylsulphamoyl chloride | HCID 83372 | — |
| Reactant | HCID 68427245 | HCID 68427245 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 86614357 | HCID 86614357 | — |
Reaction Steps
39 μL of triethylamine and 18 μL of dimethylsulfamoyl chloride were added to chloroform (1 mL) solution of 41 mg of (3S*,4S*)-3-aminomethyl-1-benzyl-4-o-tolyl-piperidine obtained in Production Example 37, and stirred at room temperature for 2.5 hours. 39 μL of triethylamine and 18 μL of dimethylsulfamoyl chloride were further added to the reaction liquid, and stirred at room temperature for 1 hour. Still further, 39 μL of triethylamine and 18 μL of dimethylsulfamoyl chloride were added to the reaction liquid, and stirred at room temperature for 1 hour. Aqueous 1 M sodium hydroxide solution was added to the reaction liquid, and extracted with ethyl acetate. The ethyl acetate layer was washed with saturated saline water, and dried with anhydrous magnesium sulfate. The solvent was evaporated off under reduced pressure, and the residue was separated and purified through preparative thin-layer chromatography (chloroform/methanol=10/1) to obtain 27 mg of the entitled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07855294B2 |
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| Source dataset | uspto-grants-2010_12 |
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| ORD ID | ord-c7dfd9597f464c439ada899b6fa29194 |
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| Source note | uspto-grants-2010_12 |
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