1,4-Dioxane → HCID 53244985, compound

Participants

Reaction Steps

To a solution of 1,1′-carbonyl-diimidazole (102 mg, 0.627 mmol) in dioxane (1 mL) was added hydroxymethylcyclopropane (55 μl, 0.68 mmol). After stirring for 15 min at ambient temperature rac-{4-[(3S,4R)-3-(3,4-dichloro-phenyl)-4-methylamino-pyrrolidine-1-carbonyl]-piperidin-1-yl}-(1-methyl-cyclopropyl)-methanone (50 mg, 0.11 mmol) was added and the solution was irradiated in the microwave for 900 s at 170° C. and 1800 s at 200° C. The reaction mixture was diluted with ethyl acetate (15 mL) and washed with water (15 mL) and brine (15 mL). The organic layers were extracted with ethyl acetate, dried over sodium sulfate and concentrated. Purification by chromatography (SiO2, ethyl acetate:methanol=100:0 to 85:15) afforded the title compound (21 mg, 34%) as a light brown oil. MS m/e: 536.4 [M]+.

Provenance & Evidence