Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 22181052 | HCID 22181052 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22181159 | HCID 22181159 | 73% |
Reaction Steps
To a suspension of 3-chloro-4-(piperidin-4-yloxy)nitrobenzene (1.00 g) obtained in reference example 8 in dichloromethane (20 ml) were added successively methanesulfonyl chloride (0.33 ml) and triethylamine (1.09 ml) with stirring under ice-cooling, and the resulting mixture was stirred at room temperature for 2 hours. After stirring, the reaction mixture was diluted with ethyl acetate, and the organic layer was washed with a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue obtained was purified by chromatography on a silica gel column using a mixed solvent of ethyl acetate and hexane (1:1) as the eluent to afford the title compound (0.96 g, yield: 73%) as a colorless amorphous solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07030138B2 |
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| Source dataset | uspto-grants-2006_04 |
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| ORD ID | ord-2e0d54aa6520414884dc40a8e5d40501 |
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| Source note | uspto-grants-2006_04 |
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