116436-03-4

基本信息
2,4-二氨基-6-乙氧基嘧啶 250MG
6-Ethoxypyrimidine-2,4-diamine
2,4-Diamino-6-ethoxy-pyrimidin
2,4-DIAMINO-6-ETHOXYPYRIMIDINE
2,4-Pyrimidinediamine, 6-ethoxy-
2,4-DIAMINO-6-ETHOXYPYRIMIDINE ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
制備方法

156-83-2

64-17-5

116436-03-4
向氫化鈉(2.77 g,69.2 mmol)的無(wú)水乙醇(150 mL)懸浮液中分批加入2,4-二氨基-6-氯嘧啶(5.0 g,34.6 mmol)。將反應(yīng)混合物加熱至回流并保持6小時(shí)。反應(yīng)完成后,冷卻至室溫,用5-6 N鹽酸的異丙醇溶液中和反應(yīng)液。減壓濃縮除去溶劑,所得殘余物通過(guò)硅膠柱色譜法(洗脫劑:二氯甲烷/甲醇=40:1,v/v)進(jìn)行純化,得到2,4-二氨基-6-乙氧基嘧啶,為白色固體(4.0 g,收率75%)。產(chǎn)物熔點(diǎn)為164-165℃。1H NMR(300 MHz,DMSO-d6,25℃):δ 6.00(s,2H,NH2),5.88(s,2H,NH2),5.03(s,1H,CH),4.13(q,J=7.1 Hz,2H,OCH2CH3),1.22(t,J=7.1 Hz,3H,OCH2CH3)。13C NMR(75 MHz,DMSO-d6,25℃):δ 170.0(C),165.9(C),162.9(C),76.1(CH),60.2(OCH2CH3),14.7(OCH2CH3)。高分辨質(zhì)譜(HRMS):計(jì)算值C6H11N4O [M+H]+ 155.09329,實(shí)測(cè)值155.09260。
參考文獻(xiàn):
[1] Bioorganic and Medicinal Chemistry, 2011, vol. 19, # 1, p. 702 - 714
[2] Patent: US2004/77859, 2004, A1. Location in patent: Page 23
[3] Organic and Biomolecular Chemistry, 2010, vol. 8, # 10, p. 2397 - 2407
[4] Journal of the American Chemical Society, 1951, vol. 73, p. 2864,2867
[5] Journal of Organic Chemistry, 2005, vol. 70, # 7, p. 2729 - 2738