Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 18423062 | HCID 18423062 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 18423141 | HCID 18423141 | — |
Reaction Steps
To a-solution of N-(4-((4-(4-aminophenyl)piperazin-1-yl)methyl)phenylmethyl)acetamide (1.8 g) and potassium carbonate (3.1 g) in a mixed solvent of water (50 ml) and ethyl acetate (50 ml) was added dropwise acetyl chloride (0.43 ml) at room temperature over 10 min. This reaction mixture was stirred at room temperature for 4 hr and poured into saturated brine, which was followed by extraction with chloroform. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate and the solvent was evaporated to give a purple solid (5.0 g). The obtained solid was subjected to column chromatography (elution solvent; chloroform:methanol=9:1) to give a pale-brown solid. The solid was recrystallized from methanol-water to give the title compound (0.75 g) as pale-red crystals, m.p.=225-226° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06455528B1 |
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| Source dataset | uspto-grants-2002_09 |
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| ORD ID | ord-a42b565241964310a2b42eb0ea719669 |
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| Source note | uspto-grants-2002_09 |
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