反应详情

To a DMF (4 mL) solution of (E)-5-chloro-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl]benzylidene)valeric acid [3-fluoro-4-(morpholin-4-yl)benzyl]amide (135 mg), sodium hydride was added at 0° C. (40% mineral oil content, 35.6 mg) was added, and the reaction solution was allowed to be warmed to room temperature and agitated for 45 minutes. The reaction solution was cooled to 0° C. after confirming disappearance of the starting materials, water and ethyl acetate were added to the reaction solution, and the organic layer was partitioned. After washed with a saturated saline solution the organic layer, it was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. 113 mg of the title compound was obtained by purifying the obtained residue by silica gel chromatography (elution solvent; ethyl acetate->ethyl acetate:ethanol 90:10). The physical properties of the compound are as follows.

1. additionwas added
2. temperatureThe reaction solution was cooled to 0° C.
3. additionwere added to the reaction solution
4. customthe organic layer was partitioned
5. washAfter washed with a saturated saline solution the organic layer, it
6. dry with materialwas dried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure