Hydrochloric Acid → HCID 10225506, compound

Participants

Reaction Steps

Sodium metal (29 mg, 1.26 mmol) was added to 1.3 mL of ethanol and stirred until homogeneous. of 1-[6-(4-Bromo-phenoxy)-pyridin-3-yl]-pyrrolidine-2,2-dicarboxylic acid diethyl ester (0.20 g, 0.42 mmol) was added, followed by urea (75 mg, 1.26 mmol) and the mixture was stirred for 5 minutes at 80° C. The mixture was cooled to ambient temperature, acidified with 1M hydrochloric acid and extracted 3× with ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated in vacuo. The residue was purified by silica gel chromatography (3:1 hexane-ethyl acetate), affording 28 mg of 1-[6-(4-Bromo-phenoxy)-pyridin-3-yl]-1,7,9-triaza-spiro[4.5]decane-2,6,8,10-tetraone as a colorless solid. HPLC Ret. time: 2.201 min; MS (APCl, m/z): 436 [M−H]−; 438 [M+H]+.

Provenance & Evidence