反应详情

A mixture of 2-(4-chloro-phenyl)-4-methyl-pentanoic acid ethyl ester (508 mg, 1.99 mmol) and urea (239 mg, 3.99 mmol) in a solution of magnesium methoxide in methanol (7.4 wt %, 4.28 mL, 2.99 mmol) was heated to reflux for 24 h. The reaction mixture was then concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 230-400 mesh, 50/50 hexanes/ethyl acetate) afforded [2-(4-chloro-phenyl)-4-methyl-pentanoyl]-urea (28.1 mg, 5.2%) as a white solid: mp 164-165° C.; EI-HRMS m/e calcd for C13H17ClN2O2 (M+) 268.0979, found 268.0972.

1. temperaturewas heated
2. temperatureto reflux for 24 h
3. concentrationThe reaction mixture was then concentrated in vacuo