反应详情

11.99 g of a 55% dispersion of sodium hydride are suspended in 40 ml of dimethylformamide and 13.04 ml of cyclopropylmethanol are added dropwise at 10° C. under a nitrogen atmosphere. The mixture is stirred for 15 minutes and then a solution of 21.16 g of 2-chloropyridin-3-ylsulfonamide in 40 ml of dimethylformamide is added dropwise. The reaction mixture is stirred for 30 minutes at 35°-40° C. and then taken up in a mixture of 275 ml of ethyl acetate, 275 ml of ice-water and 137.5 ml of 2N hydrochloric acid. The organic phase is separated and the aqueous phase is extracted with 3×100 ml of ethyl acetate. The combined organic phases are washed with 4×100 ml of water, dried, concentrated by evaporation and the residue is triturated with ether/hexane (2:1). The crystals so obtained are isolated and dried, affording 22.25 g of 2-cyclopropylmethoxypyridin-3-ylsulfonamide with a melting point of 121°-122° C.

1. stirringThe reaction mixture is stirred for 30 minutes at 35°-40° C.
2. customThe organic phase is separated
3. extractionthe aqueous phase is extracted with 3×100 ml of ethyl acetate
4. washThe combined organic phases are washed with 4×100 ml of water
5. customdried
6. concentrationconcentrated by evaporation
7. customthe residue is triturated with ether/hexane (2:1)
8. customThe crystals so obtained
9. customare isolated
10. customdried