53389-01-8

基本信息
4-氯吡啶-2,6-二羧酸二乙酯
4-氯吡啶-2,6-二甲酸二乙酯
4-氯-2,6-二吡啶二甲酸二乙酯
4-氯吡啶-2,6-二羧酸二乙酯 5G
4-chloropyridine-2,6-dicarboxylate
4-Chloro-2,6-(diethoxycarbonyl)pyridine
Ethyl 4-chloropyidine-2,6-dicarboxylate
DIETHYL 4-CHLOROPYRIDINE-2,6-DICARBOXYLATE
DIETHYL 4-CHLORO-2,6-PYRIDINEDICARBOXYLATE
Diethyl 4-Chloropyridine- 2,6-pyridinedicarboxylate
4-Chloro-2,6-pyridinedicarboxylic acid diethyl ester
2,6-Pyridinedicarboxylic acid, 4-chloro-, 2,6-diethyl ester
DIETHYL 4-CHLORO-2,6-PYRIDINEDICARBOXYLATE ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
常見問題列表

71022-75-8

64-17-5

53389-01-8
在冰浴冷卻條件下,將粗制的4-氯吡啶-2,6-二羰基二氯化物溶于二氯甲烷(100 mL)中,隨后緩慢加入吡啶(6 mL)和乙醇(5 mL)的混合溶液。反應(yīng)混合物在冰浴中攪拌5分鐘后,移去冰浴,繼續(xù)在室溫下攪拌5小時(shí)。反應(yīng)完成后,通過減壓蒸餾去除揮發(fā)性溶劑。將殘余物用1 M鹽酸(30 mL)和飽和氯化鈉水溶液(50 mL)的混合液洗滌,隨后用二氯甲烷(200 mL)萃取。合并有機(jī)相,用無水硫酸鎂干燥,過濾后減壓濃縮。粗產(chǎn)物通過硅膠快速柱色譜法純化,采用乙酸乙酯-己烷(1:4,隨后調(diào)整為1:3)作為洗脫劑,最終得到4-氯-2,6-吡啶二羧酸二乙酯(800 mg,產(chǎn)率62%)。產(chǎn)物經(jīng)1H NMR(DMSO-d6)表征:δ 1.36(t,6H,J = 7.1 Hz,CH3),3.33(s,3H,CH3),4.40(q,4H,J = 7.1 Hz,CH2),8.31(s,2H,Ar)。
參考文獻(xiàn):
[1] Patent: US2004/198728, 2004, A1. Location in patent: Page/Page column 8
[2] Canadian Journal of Chemistry, 1991, vol. 69, # 7, p. 1107 - 1116
[3] Bioorganic and Medicinal Chemistry Letters, 2005, vol. 15, # 21, p. 4703 - 4707
[4] Chemical Communications, 2014, vol. 50, # 71, p. 10323 - 10326