Cyanamide → HCID 178480761, Verbindung

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.

1. temperatureThe mixture was cooled down to room temperature
2. extractionextracted with DCM (10 mL)
3. additionNaOH 2N was added to pH>11
4. extractionThe aqueous phase was extracted with Et2O (3×10 mL)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe residue was crystallized from diethyl ether

ORD-Eintrag

ord-8aca38b3ccb64ca4999b051da1f10def

Quelldatensatz

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08614220B2