5395-50-6
5395-50-6 結(jié)構(gòu)式
基本信息
1,3,4,6-四羥甲基甘脲
四羥甲基咪唑雜[4,5-D]咪唑-2,5[1H,2H]-二酮
四氫-1,3,4,6-四(羥甲基)咪唑并[4,5-D]咪唑-2,5(1H,3H)-二酮
Tetramethylol acetylenediurea
Tetramethylol acetylene diuriene
Tetrakis (hydroxy methy1) glycoluril
1,3,4,6-tetramethylol-3a,6a-dihydroimidazo[4,5-d]imidazole-2,5-quinone
1,3,4,6-Tetrakis(hydroxymethyl)octahydroimidazo[4,5-d]imidazole-2,5-dione
1,3,4,6-Tetrakis-hydroxymethyl-tetrahydro-imidazo(4,5-d)imidazole-2,5-dione
1,3,4,6-tetrakis(hydroxymethyl)-3a,6a-dihydroimidazo[4,5-d]imidazole-2,5-dione
Tetrahydro-1,3,4,6-tetrakis(hydroxymethyl)imidazo[4,5-d]imidazol-2,5(1H,3H)-dion
1,3,4,6-Tetrakis(hydroxyMethyl)tetrahydroiMidazo[4,5-d]iMidazole-2,5(1H,3H)-dione
物理化學(xué)性質(zhì)
制備方法
50-00-0
496-46-8
5395-50-6
在配備有機(jī)械攪拌器、溫度計(jì)和回流冷凝器的合適反應(yīng)容器中，加入688份（10mol）44%甲醛水溶液，并用22份0.5N NaOH溶液調(diào)節(jié)pH至8.7。將反應(yīng)體系溫度維持在40℃，隨后向其中加入284份（2mol）甘脲。反應(yīng)過(guò)程中，溫度逐漸升至55℃，此時(shí)大部分甘脲溶解。約15分鐘后，用5份0.5N NaOH溶液將反應(yīng)體系的pH調(diào)節(jié)至8.0，得到澄清的淺黃色溶液。將此溶液在50℃下進(jìn)行減壓蒸餾，除去水分，直至反應(yīng)容器內(nèi)剩余物約為640份。將濃縮后的糖漿狀產(chǎn)物倒入800份甲醇中，析出白色結(jié)晶沉淀。經(jīng)過(guò)濾和干燥后，得到483份（收率92%）1,3,4,6-四(羥甲基)四氫咪唑并[4,5-d]咪唑-2,5(1H,3H)-二酮，熔點(diǎn)為132℃~136℃。
參考文獻(xiàn)：
[1] Patent: WO2014/166347, 2014, A1. Location in patent: Page/Page column 14
[2] Patent: WO2015/143974, 2015, A1. Location in patent: Page/Page column 15; 16
[3] Chemistry of Heterocyclic Compounds, 2006, vol. 42, # 3, p. 365 - 376
[4] Russian Journal of Applied Chemistry, 2016, vol. 89, # 1, p. 132 - 139
[5] Zh. Prikl. Khim. (S.-Peterburg, Russ. Fed.), 2016, vol. 89, # 1, p. 103 - 111,9