1865-11-8

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879-65-2

1865-11-8
將2-喹喔啉羧酸(1.0 g,5.7 mmol,1.0 eq.)溶解于20 mL甲醇中,緩慢加入亞硫酰氯(1.25 mL,17.2 mmol,3.0 eq.)。將反應(yīng)混合物加熱回流3小時。反應(yīng)完成后,冷卻至室溫,減壓濃縮除去溶劑。殘余物用乙酸乙酯萃取,水洗,分液,有機相用無水硫酸鈉干燥。過濾后,減壓濃縮有機相。通過硅膠柱色譜純化(洗脫劑:石油醚/乙酸乙酯=5:1),得到淺黃色固體產(chǎn)物喹喔啉-2-甲酸甲酯(1.01 g,產(chǎn)率93.5%)。
參考文獻:
[1] Advanced Synthesis and Catalysis, 2009, vol. 351, # 16, p. 2549 - 2552
[2] Patent: CN107383024, 2017, A. Location in patent: Paragraph 0395
[3] Patent: WO2018/116072, 2018, A1. Location in patent: Page/Page column 74
[4] Supramolecular Chemistry, 2015, vol. 27, # 11-12, p. 780 - 786
[5] Tetrahedron, 2016, vol. 72, # 10, p. 1375 - 1380