3099-29-4

基本信息
2-Chloromethyl-6-methylpyridine
2-(Chloromethyl)-6-methylpyridin
Pyridine, 2-(chloromethyl)-6-methyl-
2-(chloromethyl)-6-methylpyridine(SALTDATA: HCl)
2-(CHLOROMETHYL)-6-METHYLPYRIDINE ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

1122-71-0

3099-29-4
制備例10-1-1 2-氯甲基-6-甲基吡啶:將(6-甲基吡啶-2-基)甲醇(1.44 g,11.7 mmol)溶于二氯甲烷(20 mL)中,加入亞硫酰氯(1.45 mL,19.9 mmol)。將反應(yīng)混合物在回流條件下攪拌40分鐘。反應(yīng)完成后,將反應(yīng)液冷卻至室溫,隨后在減壓下濃縮。將濃縮后的殘余物分配于碳酸氫鈉溶液和乙醚之間。分離有機(jī)層,減壓濃縮,所得殘余物通過硅膠柱色譜法(洗脫劑:乙酸乙酯)純化,得到目標(biāo)產(chǎn)物2-氯甲基-6-甲基吡啶(1.42 g,收率85.8%)。1H-NMR (DMSO-d6) δ (ppm): 2.47 (3H, s), 4.72 (2H, s), 7.22 (1H, d, J = 7.6 Hz), 7.33 (1H, d, J = 7.6 Hz), 7.72 (1H, dd, J = 7.6, 7.6 Hz)。
參考文獻(xiàn):
[1] Journal of the American Chemical Society, 2005, vol. 127, # 29, p. 10197 - 10204
[2] Patent: US2009/82403, 2009, A1. Location in patent: Page/Page column 64
[3] Patent: US2007/105904, 2007, A1. Location in patent: Page/Page column 61
[4] Chinese Chemical Letters, 2018, vol. 29, # 11, p. 1637 - 1640
[5] Chemistry Letters, 1998, # 9, p. 915 - 916