反应详情

To a solution of 2-(4-nitro-1H-pyrazol-1-yl)ethanamine hydrochloride (1.0 g) obtained in Step B of Example 348 in tetrahydrofuran (30 mL) were added triethylamine (2.2 mL) and methanesulfonyl chloride (0.60 mL) in an ice bath, and the mixture was stirred at room temperature for 3 hr. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with water and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was recrystallized (hexane/ethyl acetate) to give the title compound (880 mg).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe obtained organic layer was washed with water and saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. customthe solvent was evaporated under reduced pressure
5. customThe residue was recrystallized (hexane/ethyl acetate)