14161-11-6

基本信息
3,4,5-三氯噠嗪
3,4,5-三氯噠嗪(CAS號(hào):14161-11-6)
3,4,5-TrichL
Einecs 238-006-2
3,4,5-Trichlorpyridazin
3,4,5-TRICHLOROPYRIDAZINE
Pyridazine,3,4,5-trichloro-
3,4,5-Trichloro-1,2-diazine
3,4,5-TRICHLOROPYRIDAZINE 98%
3,4,5-TRICHLOROPYRIDAZINE ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

932-22-9

14161-11-6
以4,5-二氯噠嗪-3(2H)-酮為原料合成3,4,5-三氯噠嗪的一般步驟:將4,5-二氯-3-羥基噠嗪(25 g,151 mmol)與磷酰氯(80 mL)混合,在回流條件下(120℃)攪拌反應(yīng)24小時(shí)。反應(yīng)完成后,通過(guò)減壓蒸餾除去過(guò)量的磷酰氯。將殘余物冷卻至-78℃,保持5-10分鐘后,緩慢加入冰(300 mL)。隨后,將反應(yīng)體系從-78℃浴轉(zhuǎn)移至0℃浴,并逐漸升溫至室溫。待冰完全融化后,將析出的白色固體粉碎,并將混合物繼續(xù)攪拌過(guò)夜。通過(guò)過(guò)濾收集固體產(chǎn)物,用水洗滌并干燥,得到中間體I-09(26.105 g,收率94%),為白色固體。HPLC-MS(方法4)分析結(jié)果:保留時(shí)間(Rt)= 3.3分鐘,[M + H]+ m/z = 183。
參考文獻(xiàn):
[1] Patent: WO2013/4984, 2013, A1. Location in patent: Page/Page column 70
[2] Patent: US2014/171435, 2014, A1. Location in patent: Paragraph 0451; 0452; 0453
[3] Patent: WO2015/189744, 2015, A1. Location in patent: Page/Page column 66-67
[4] Patent: US6800758, 2004, B1. Location in patent: Page column 12
[5] Journal of Organic Chemistry, 2014, vol. 79, # 21, p. 10311 - 10322