13621-50-6

基本信息
硫代氨基甲酰乙酸乙酯
3-氨基-3-硫代丙酸乙酯
3-氨基-3-硫氧代丙酸乙酯
3-氨基-3-硫代甲?;嵋阴?/span>
(Ethoxycarbonyl)thioacetamide
ETHYL 3-AMINO-3-THIOXOPROPANOATE
alpha-Ethoxycarbonylthioacetamide
ETHYL 3-1AMINO-3-THIOXOPROPANOATE
THIOCARBAMOYL ACETIC ACID ETHYL ESTER
Propanoic acid,3-amino-3-thioxo-, ethyl ester
ETHYL 3-AMINO-3-THIOXOPROPANOATE ISO 9001:2015 REACH
THIOCARBAMOYL ACETIC ACID ETHYL ESTER
ETHYL 3-AMINO-3-THIOXOPROPANOATE
物理化學(xué)性質(zhì)
制備方法

105-56-6

13621-50-6
步驟A:在氮?dú)獗Wo(hù)下,將氰基乙酸乙酯(4.7 mL,44.3 mmol)溶解于吡啶/三乙胺混合溶劑(500 mL,1:1 v/v)中。向該溶液中緩慢通入硫化氫氣體(H2S)直至飽和。將反應(yīng)混合物加熱至60℃并攪拌18小時(shí)。反應(yīng)完成后,在減壓下蒸除溶劑。將殘余物用乙酸乙酯(EtOAc)和稀鹽酸水溶液進(jìn)行萃取分離。有機(jī)層用無(wú)水硫酸鎂(MgSO4)干燥,過(guò)濾后減壓濃縮。通過(guò)過(guò)濾去除殘留的固體雜質(zhì),得到3-氨基-3-硫代丙酸乙酯(6.25 g,96%收率),為橙色油狀物。產(chǎn)物經(jīng)1H NMR(500 MHz,CDCl3)表征:δ 8.92(1H,寬單峰),7.75(1H,寬單峰),4.21(2H,四重峰,J = 7 Hz),3.82(2H,單峰),1.29(3H,三重峰,J = 7 Hz)。
參考文獻(xiàn):
[1] Patent: WO2013/101974, 2013, A1. Location in patent: Paragraph 00704; 00705
[2] Patent: US9617268, 2017, B2. Location in patent: Page/Page column 347; 348
[3] Synlett, 2009, # 14, p. 2338 - 2340
[4] Phosphorus, Sulfur and Silicon and the Related Elements, 1994, vol. 96, # 1-4, p. 325 - 326
[5] Helvetica Chimica Acta, 1948, vol. 31, p. 1342,1348