1658-42-0

基本信息
2-吡啶基乙酸甲酯
吡啶-2-乙酸甲酯
2-吡啶乙酸甲酯 1KG
2-吡啶乙酸甲酯MFCD00006358
METHYLPYRIDYL-2 ACETATE
METHYL 2-PYRIDYLACETATE
METHYL 2-PYRIDINEACETATE
Methyl 2-pyridinylacetate
Methyl pyridine-2-acetate
METHYL PYRIDIN-2-YLACETATE
Methyl 2-pyridylacetate,98%
methyl 2-(pyridin-2-yl)acetate
Methyl 2-pyridylacetate, GC 98%
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

67-56-1

16179-97-8

1658-42-0
以甲醇和2-吡啶乙酸鹽酸鹽為原料合成2-吡啶乙酸甲酯的一般步驟如下:參照文獻(xiàn)方法制備目標(biāo)化合物。將2.00 g 2-吡啶乙酸鹽酸鹽(11.5 mmol,1.00當(dāng)量)與14 mL甲醇加入圓底燒瓶中。將反應(yīng)體系冷卻至0℃,緩慢滴加2.90 mL三甲基氯硅烷(23.0 mmol,2.00當(dāng)量)。待滴加完畢后,將反應(yīng)混合物逐漸升溫至室溫并攪拌反應(yīng)過夜。反應(yīng)完成后,通過旋轉(zhuǎn)蒸發(fā)儀減壓除去溶劑。向殘余固體中緩慢加入40 mL飽和碳酸氫鈉水溶液進(jìn)行中和。隨后,用二氯甲烷(4×40 mL)萃取水相,合并有機(jī)相并用無水硫酸鈉干燥。過濾后,減壓濃縮有機(jī)相,得到粗產(chǎn)物2-吡啶乙酸甲酯(1.73 g,11.47 mmol,收率定量),為透明油狀物。通過對(duì)比化合物的光譜數(shù)據(jù)與文獻(xiàn)報(bào)道數(shù)據(jù)確認(rèn)產(chǎn)物結(jié)構(gòu)。
參考文獻(xiàn):
[1] Tetrahedron, 2011, vol. 67, # 24, p. 4435 - 4441
[2] Patent: WO2017/87667, 2017, A1. Location in patent: Paragraph 0069
[3] Journal of the American Chemical Society, 2015, vol. 137, # 32, p. 10246 - 10253
[4] Journal of Organic Chemistry, 2001, vol. 66, # 20, p. 6595 - 6603