Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | HCID 9822304 | HCID 9822304 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 9824265 | HCID 9824265 | 92.7% |
Reaction Steps
A mixture of N,N-dimethyl-2-[6-phenyl-2-(4-trifluoromethyl-phenyl)-4-pyrimidinylamino]acetamide (15.9 g), N-chlorosuccinimide (6.4 g) and acetic acid (80 ml) is stirred at 90° C. for 1.5 hour. The reaction mixture is concentrated under reduced pressure, and water and chloroform are added to the residue. The mixture is neutralized with an aqueous sodium hydroxide solution (1 mol/L), and the chloroform layer is separated. The chloroform layer is dried over anhydrous sodium sulfate, concentrated under reduced pressure, and the residue is purified by silica gel column chromatography (eluent: chloroform), and recrystallized from ethanol to give the desired compound (16 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06620817B1 |
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| Source dataset | uspto-grants-2003_09 |
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| ORD ID | ord-6695321df8184c1eaca4dba15c12fe03 |
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| Source note | uspto-grants-2003_09 |
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