反应详情

0.5 ml of a 0.3 M tetrahydrofuran solution of methyl magnesium bromide was added to a 3 ml tetrahydrofuran solution of 0.050 g of t-butyl 4-[1-(2-butynyl)-5-ethoxycarbonyl-4-formyl-1H-imidazol-2-yl]piperazine-1-carboxylate at −70° C. under a nitrogen atmosphere, and the mixture was allowed to warm to room temperature. 10 ml of a 5% aqueous ammonium chloride solution was added to this solution, and the mixture was extracted with 30 ml of ethyl acetate. The organic layer was washed successively with 10 ml of water and 10 ml of a saturated sodium chloride solution, and then dried over magnesium sulfate. The organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography. Thus, 0.049 g of the title compound was obtained from the fraction eluted with ethyl acetate-hexane (1:1).

1. extractionthe mixture was extracted with 30 ml of ethyl acetate
2. washThe organic layer was washed successively with 10 ml of water and 10 ml of a saturated sodium chloride solution
3. dry with materialdried over magnesium sulfate
4. concentrationThe organic layer was concentrated under reduced pressure
5. customThe residue was purified by silica gel column chromatography