34107-46-5

基本信息
6-甲基-3-甲醇吡啶
6-甲基-3-羥甲基吡啶
(6-甲基-3-吡啶基)甲醇
(6-甲基吡啶-3-基)甲醇
2-甲基-5-(羥甲基)吡啶
6-Methylpyridine-3-methanol
6-Methyl-3-PyridineMethanol
(6-Methyl-3-pyridyl)methanol
6-(Methylpyridin-3-yl)methano
3-Pyridinemethanol, 6-methyl-
(6-methyl-3-pyridinyl)methanol
6-Methyl-3-pyridinemethanol >
5-(Hydroxymethyl)-2-methylpyridine
5-Hydroxymethyl-2-methylpyridine 97%
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

5470-70-2

34107-46-5
以6-甲基煙酸甲酯為原料合成6-甲基-3-甲醇吡啶的一般步驟:在-5℃下,向攪拌的6-甲基煙酸甲酯(21g; 140mmol; 1當(dāng)量)的無水THF(150mL)溶液中緩慢滴加1M LiAlH4的THF溶液(210mL; 210mmol; 1.5當(dāng)量)。滴加完畢后,將反應(yīng)混合物在23℃下繼續(xù)攪拌2小時。隨后,將混合物冷卻至-10℃,并用硫酸鈉十水合物和乙酸乙酯小心淬滅反應(yīng),直至停止產(chǎn)生氣泡。將混合物通過硅藻土墊過濾,濾液經(jīng)減壓濃縮至干,得到6-甲基-3-甲醇吡啶(17g,產(chǎn)率100%)。產(chǎn)物經(jīng)1H NMR(DMSO-d6)表征:δ 8.37(s,1H),7.59(dd,1H,J = 2,8Hz),7.19(d,1H,J = 8Hz),5.22(t,1H,J = 6Hz),4.47(d,2H,J = 6Hz),2.45(s,3H)。
參考文獻(xiàn):
[1] Patent: WO2015/95128, 2015, A1. Location in patent: Paragraph 0152; 0155; 0156
[2] Organic Preparations and Procedures International, 2015, vol. 47, # 3, p. 220 - 226
[3] Patent: US2005/124586, 2005, A1. Location in patent: Page/Page column 7
[4] Journal of the Chemical Society. Perkin Transactions 2, 2002, # 5, p. 928 - 937
[5] Patent: WO2018/165718, 2018, A1. Location in patent: Page/Page column 100; 101; 102