反应详情

To a tetrahydrofuran (THF) (3.0 ml) solution of [4-(2,2,2-trifluoro-1,1-dimethylethyl)phenoxy]acetic acid (157 mg, 0.6 mmol) was added 2-chloro-1,3-dimethylimidazolinium chloride (CDI) (97 mg, 0.6 mmol) at room temperature and the mixture was stirred for 2 hours, followed by additional stirring for 10 hours with triethylamine (0.33 ml) and N-[4-(aminomethyl)-2-fluorophenyl]methanesulfonamide hydrochloride (122 mg, 0.48 mmol). The reaction was partitioned with water and methylene dichloride and the organic layer was separated, dried over sodium sulfate. After filtration to separate solvent and sodium sulfate, the solvent was removed under reduced pressure to give a residue, which was applied to a silica gel chromatography column and eluted with a volume mixture of methylene dichloride and methanol (5/1 to 5/2) to furnish 62.9 mg (28% yield) of the title compound as colorless oil.

1. customThe reaction was partitioned with water and methylene dichloride
2. customthe organic layer was separated
3. dry with materialdried over sodium sulfate
4. filtrationAfter filtration
5. customto separate solvent and sodium sulfate
6. customthe solvent was removed under reduced pressure
7. customto give a residue, which
8. washeluted with a volume mixture of methylene dichloride and methanol (5/1 to 5/2)