Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyanamide | HCID 9864 | — |
| Reactant | 5-(4-Methylpiperazin-1-yl)-2-trifluoromethoxyphenylamine | HCID 24994142 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178480761 | HCID 178480761 | 76% |
Reaction Steps
To a solution of 5-(4-methyl-piperazin-1-yl)-2-trifluoromethoxy-phenylamine (275 mg, 1 mmol) in HCl 6N (1 mL), cyanamide (336 mg, 8.0 mmol) was added and the reaction was stirred at 60° C. for 1 h. The mixture was cooled down to room temperature, diluted with water (3 mL), extracted with DCM (10 mL). NaOH 2N was added to pH>11. The aqueous phase was extracted with Et2O (3×10 mL), dried over sodium sulfate and concentrated. The residue was crystallized from diethyl ether to give the title compound (240 mg, 76% yield) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08614220B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-8aca38b3ccb64ca4999b051da1f10def |
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| Source note | uspto-grants-2013_12 |
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