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波普医药正在热销:

别名:6-甲基吡啶-3-磺酰氯
英文名称:6-methylpyridine-3-sulfonyl chloride
分子式:c6h6clno2s
cas no.:478264-00-5
分子量:191.63534
结构式:

规格:95%

用途:基础原料、有机中间体、医药中间体

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hydrogenchloride; sodium nitrite; hydrogenchloride; sodium hydrogensulfite; copper(ii) sulfate; water; water;

 

reactants are commercially availlable.

takeda pharmaceutical company limited, us2007/60623, a1, (2007) reference example 186 6-methylpyridin-3-ylsulfonyl chloride; to a mixture of 6-methylpyridine-3-amine (449 mg) and concentrated hydrochloric acid (5 ml) was added a solution of sodium nitrite (857 mg) in water (2 ml) at 0°c., and the mixture was stirred at the same temperature for 10 min. to the mi xture was added a solution of concentrated hydrochloric acid (2.5 ml), copper sulfate (69 mg) and so dium hydrogen sulfite (5.08 g) in water (8 ml) at 0°c., and the mixture was stirred at room tempera ture for 30 min. the reaction mixture was extracted with ethyl acetate. the extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. the residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=10:1) to gi ve the title compound as a pale-yellow solid (yield 0.12 g, 15percent). 1h-nmr (cdcl3)delta: 2.73 (3h, s), 7.40-7.43 (1h, m), 8.16-8.20 (1h, m), 9.11-9.12 (1h, m).

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