Sulfamide derivative, preparation method and application thereof in resisting tumor
A technology of derivatives and sulfonamides, which is applied in the field of sulfonamide derivatives, preparation and anti-tumor applications, can solve problems such as interference and achieve good activity
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Embodiment 1
[0020] Example 1: Synthesis of 1-((4,5-dihydro-1H-imidazol-1-yl)sulfonyl)pyrrolidine-3-carbonyl chloride
[0021]
[0022] A solution of pyrrolidine-3-carbonyl chloride (16.8ml, 0.2mol) in anhydrous toluene (40ml) was added dropwise to 4,5-dihydro-1H-imidazole-1-sulfonyl chloride (33.72g, 0.2mol) In a cold (-10°C) solution in toluene (30ml) such that the internal temperature does not exceed -5°C. Once the addition was complete, the mixture was stirred at -5°C for thirty minutes before water (50ml) was added. The layers were separated, the organic layer was washed with HCl (2mol / l, 50ml), washed with anhydrous MgSO 4 Drying and evaporation in vacuo gave a clear oil (9.6g). The oil is a 2:1 mixture of the desired sulfamoyl chloride and 1-((4,5-dihydro-1H-imidazol-1-yl)sulfonyl)pyrrolidine-3-carbonyl chloride. 42.4 g of 1-((4,5-dihydro-1H-imidazol-1-yl)sulfonyl)pyrrolidine-3-carbonyl chloride was obtained by column chromatography with a yield of 80%. 1 H-NMR (400 MHz, CDCl...
Embodiment 2
[0023] Example 2: N-(2,6-dichloropyridin-4-yl)-1-((4,5-dihydro-1H-imidazol-1-yl)sulfonyl)pyrrolidine-3-carboxamide synthesis
[0024]
[0025] 1-((4,5-Dihydro-1H-imidazol-1-yl)sulfonyl)pyrrolidine-3-carbonyl chloride (53.14 g, 0.2 mol) was dissolved in anhydrous CH 2 Cl 2 (36 mL) was carefully added to 2,6-dichloro-4-aminopyridine (32.60 g, 0.2 mol) and triethylamine (27 mL) in anhydrous CH at 0 °C 2 Cl 2 (90mL) solution). The reaction mixture was stirred in an ice bath for 1 hour, then allowed to warm to room temperature and stirred overnight. Add cold water (100 mL), and separate the CH from the aqueous solution 2 Cl 2 layer. Organic phase with saturated NaHCO 3 solution (2 x 40 mL) and washed with water, with anhydrous MgSO 4 Drying, filtration and concentration gave the crude product, which was recrystallized from ethyl acetate / n-hexane (1:5) to give N-(2,6-dichloropyridin-4-yl)-1- ((4,5-Dihydro-1H-imidazol-1-yl)sulfonyl)pyrrolidine-3-carboxamide 66.68g, yield...
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