Dichloromethane → HCID 69279870, compound

Participants

Reaction Steps

4-Tert-butylphenyl isocyanate (0.218 ml, 1.24 mmol), dissolved in abs. DCM (5 ml), was added dropwise to a solution of compound Y (286 mg, 1.24 mmol) in abs. DCM (10 ml) at RT within 20 min. After stirring for 3.5 h at RT, the solution was washed with 10% citric acid solution (1×10 ml) and water (1×10 ml), dried and concentrated. The colourless oil obtained (742 mg) contained few impurities. The oil was mixed with diethyl ether (10 ml) and stored at 5° C. The precipitated solid was removed by suction-filtration and washed with diethyl ether (5 ml). The desired product 3-benzyl-1-oxa-2,8-diazaspiro[4.5]dec-2-ene-8-carboxylic acid-(4-tert-butylphenyl)amide was obtained in a yield of 73% (369 mg) having a melting point of 137-139° C.

Provenance & Evidence