反应详情

5.59 g of sodium hydrosulfide hydrate (purity: 70%, 69.8 mmoles) was added, at room temperature, to a solution of 6.84 g (35.8 mmoles) of 5,5-dimethyl-3-ethanesulfonyl-2-isoxazoline dissolved in 200 ml of N,N-dimethylformamide. The mixture was stirred for 1 hour. To the reaction mixture, were added 4.94 g (35.8 mmoles) of anhydrous potassium carbonate, 5.51 g (35.8 mmoles) of Rongalit and further 9.46 g (34.1 mmoles) of 4-bromomethyl-5-chloro-1-methyl-3-trifluoromethyl-1H-pyrazole. The resulting mixture was stirred at room temperature over one night to give rise to a reaction. After confirmation of the completion of the reaction, the reaction mixture was poured into water, followed by extraction with ethyl acetate. The resulting organic layer was washed with water and an aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein. The residue was purified by silica gel column chromatography to obtain 8.97 g (yield: 80.3%) of 3-(5-chloro-1-methyl-3-trifluoromethylpyrazol-4-ylmethylthio)-5,5-dimethyl-2-isoxazoline.

1. stirringThe resulting mixture was stirred at room temperature over one night
2. customto give rise
3. customto a reaction
4. customAfter confirmation of the completion of the reaction
5. extractionfollowed by extraction with ethyl acetate
6. washThe resulting organic layer was washed with water
7. dry with materialan aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate
8. distillationThe resulting solution was subjected to vacuum distillation
9. customto remove the solvent
10. customThe residue was purified by silica gel column chromatography