反应详情

温度

100 °C

A mixture of 2.53 g (0.01 mol) of ethyl 4-chloro-1,3-dimethyl-1H pyrazolo[3,4-b]pyridine-5-carboxylate, 1.89 g (0.01 mol) of N-methyl-4-fluorobenzenesulfonamide, 6.91 g (0.05 mol) of anhydrous K2CO3, 0.143 g of 18-crown-6 and 70 ml of anhydrous 1-methyl-2-pyrrolidinone was stirred and heated at 100° C. for 17 hours. The solvent was removed under vacuum and water added to the residue. The mixture was extracted with CH2Cl2, and the extract washed with H2O, brine and dried (Na2SO4). The solution was filtered through a pad of hydrous magnesium silicate and the filtrate concentrated to dryness under vacuum to give 4.98 g of an oil. This oil was chromatographed on a silica gel column with ethyl acetate-hexane(2:3) as solvent to give 3.15 g of solid, mp 107-109° C.

1. customThe solvent was removed under vacuum and water
2. additionadded to the residue
3. extractionThe mixture was extracted with CH2Cl2
4. washthe extract washed with H2O, brine
5. dry with materialdried (Na2SO4)
6. filtrationThe solution was filtered through a pad of hydrous magnesium silicate
7. concentrationthe filtrate concentrated to dryness under vacuum