5264-35-7

基本信息
2-甲氧基-1-吡咯啉
2-甲氧基-1-吡咯烷
2-甲氧基-4,5-二氫-3H-吡咯
5-甲氧基-3,4-二氫-2H-吡咯
2H-吡咯,3,4-二氫-5-甲氧基-
2-methoxypyrrole
AKOS BBS-00007016
2-METHOXY-1-PYRROLINE
Tipiracil Impurity 16
Piracetam EP Impurity 5
4,5-Dihydro-2-methoxy-3H-pyrrole
5-METHOXY-3,4-DIHYDRO-2H-PYRROLE
3,4-dihydro-5-methoxy-2H-Pyrrole
2-methoxy-4,5-dihydro-3H-pyrrole
物理化學(xué)性質(zhì)
制備方法

616-45-5

77-78-1

5264-35-7
以2-吡咯烷酮和硫酸二甲酯為原料合成2-甲氧基-1-吡咯烷的一般步驟:將23 mL(1當(dāng)量)硫酸二甲酯緩慢滴加到20.03 g(0.235 mol)2-吡咯烷酮溶于85 mL苯的溶液中,隨后將反應(yīng)混合物加熱至70℃并保持回流3小時。反應(yīng)完成后,將混合物冷卻至室溫,然后加入19 mL 15 N的氫氧化鈉溶液。將反應(yīng)混合物轉(zhuǎn)移至分液漏斗中,水相用苯萃取三次。合并有機相,用無水硫酸鈉干燥,隨后在減壓下蒸發(fā)溶劑。殘余物通過真空蒸餾純化,得到無色液體的2-甲氧基-1-吡咯烷,產(chǎn)率為58%。產(chǎn)物沸點為37℃(10^-2 mbar)。1H NMR(CDCl3, 100 MHz)數(shù)據(jù)如下:δ 1.97(m, 2H), 2.41(t, 2H), 3.61(t, 2H), 3.75(s, 3H)。
參考文獻:
[1] Arkivoc, 2016, vol. 2016, # 5, p. 118 - 141
[2] Journal of Organic Chemistry, 1995, vol. 60, # 9, p. 2912 - 2915
[3] Organic Preparations and Procedures International, 1992, vol. 24, # 2, p. 147 - 158
[4] Journal of Medicinal Chemistry, 2001, vol. 44, # 10, p. 1588 - 1593
[5] Journal of Medicinal Chemistry, 2007, vol. 50, # 25, p. 6307 - 6315