Tetrahydrofuran → HCID 57495633, compound

Participants

Reaction Steps

1.62 g (9.08 mmol) of 1-Cyclopropylamino-cycloheptanecarbonitrile and the crude 4-Isocyanato-benzoic acid ethyl ester in 15 ml THF were stirred for 3 h at RT and then 3.8 ml (27.3 mmol) of triethylamin was added. The stirring was continued for 24 h and then the reaction mixture was concentrated under reduced pressure to dryness. To the dry residue was added 17 ml of 2N HCl and 33 ml of Ethanol and the whole was refluxed for 1 h. The reaction mixture was taken up in EtOAc and washed with water. The organic layers were concentrated under reduced pressure and the crude product was purified by chromatography over silica gel with EtOAc/Heptan 1:2 to give 265 mg of pure 4-(1-Cyclopropyl-2,4-dioxo-1,3-diaza-spiro[4.6]undec-3-yl)-benzoic acid ethyl ester. MS (ESI): 357.3 (MH+).

Provenance & Evidence