反应详情

A suspension of 5-(2-bromoethyl)benzofurazan (0.39 g, 1.72 mmol), 3,4-dihydro-6-methanesulfonamidospiro[(2H)-1-benzopyran-2,4'-piperidine]-4-one hydrochloride (0.24 g, 0.69 mmol) and sodium bicarbonate (0.21 g, 2.55 mmol) in ethanol (13.2 ml) was heated at reflux temperature for 24 hr. Solvent evaporation and chromatography (silica gel, chloroform-methanol-ammonium hydroxide, 97/3/0.3) gave an oil; conversion to the hydrochloride gave the hydrochloride (0.14 g, 41%); mp>250° C. Anal. Calcd for C22H24N4O3 ·HCl C, 53.59; H, 5.12, N, 11.37. Found: C, 53.55; H, 5.15; N, 11.12.

1. temperaturewas heated
2. temperatureat reflux temperature for 24 hr
3. customSolvent evaporation and chromatography (silica gel, chloroform-methanol-ammonium hydroxide, 97/3/0.3)
4. customgave an oil