反应详情

In N,N-dimethylformamide (1 ml), 1-[(6-chloronaphthalen-2-yl)sulfonyl]-6-methoxycarbonyl-1,2,3,4-tetrahydropyrazine (60 mg) and p-nitrophenyl 4-(pyridin-4-yl)benzoate (52 mg) were dissolved, followed by the addition of sodium hydride (60% in oil, 7.20 mg) under ice cooling. The resulting mixture was stirred for 1 hour. Water and ethyl acetate were added to the reaction mixture to separate the organic layer. The organic layer was dried over anhydrous magnesium sulfate and the solvent was concentrated under reduced pressure. The residue was purified by chromatography on a silica gel column (ethyl acetate:hexane=2:1), followed by dissolution in ethanol. To the resulting solution, 1N aqueous hydrochloric acid in ethanol was added and the resulting mixture was concentrated, whereby the title compound (58 mg, 60%) was obtained as pale yellow powder.

1. customto separate the organic layer
2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
3. concentrationthe solvent was concentrated under reduced pressure
4. customThe residue was purified by chromatography on a silica gel column (ethyl acetate:hexane=2:1)
5. dissolutionfollowed by dissolution in ethanol
6. additionTo the resulting solution, 1N aqueous hydrochloric acid in ethanol was added
7. concentrationthe resulting mixture was concentrated