Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyanamide | HCID 9864 | — |
| Reactant | 4-(4-Methyl-piperazin-1-yl)-2-trifluoromethoxy-phenylamine | HCID 66678306 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178480751 | HCID 178480751 | 76% |
Reaction Steps
To a solution of 4-(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 hours. The mixture was cooled down to room temperature, diluted with H2O (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 Na2SO4 and concentrated. The residue was crystallized from Et2O to give the title compound (240 mg, 76% yield) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09333205B2 |
|---|
| Source dataset | uspto-grants-2016_05 |
|---|
| ORD ID | ord-07e2fa86e36e48c88e34929cd427c5b9 |
|---|
| Source note | uspto-grants-2016_05 |
|---|