Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Magnesium | HCID 5462224 | — |
| Reactant | HCID 86709392 | HCID 86709392 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 70874708 | HCID 70874708 | — |
Reaction Steps
Magnesium (1.83 g, 75.0 mmol) was added to a methanol solution (50 ml) of 1-{1-methyl-1-[4-(4-trifluoromethylbenzyloxy)phenyl]ethyl}-4-(toluene-4-sulfonyl]piperazine (2.67 g, 5.0 mmol) and stirred at 60° C. After hours, magnesium (0.61 g, 25.1 mmol) was added thereto and further stirred. After 1 hour, heating was stopped and the solvent was distilled off. Ice and 10% hydrochloric acid (100 ml) were added to the residue and stirred. Ethyl acetate was added and further stirred. The mixture was separated into layers, and the water layer was made basic using a 25% sodium hydroxide aqueous solution. Ethyl acetate was added to the mixture, followed by stirring. The mixture was filtered through Celite to remove the insoluble matter. The filtrate was subjected to extraction with ethyl acetate. The organic layer was dried over sodium sulfate. After removing the desiccant by filtration, the solvent was distilled off to afford the title compound as a slightly yellow oil (1.05 g, 55%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09051333B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-6352c6238f524a3cb21859e4e6b1f1d2 |
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| Source note | uspto-grants-2015_06 |
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