54664-55-0
54664-55-0 結(jié)構(gòu)式
基本信息
4-氯-6,7-二氫-5H-環(huán)戊二烯并[B]吡啶
6,7-Dihydro-5H-[1]pyrindin-4-ylaMine
5H-1-Pyrindine, 4-chloro-6,7-dihydro-
4-CHLORO-6,7-DIHYDRO-5H-CYCLOPENTA[B]PYRIDINE
5H-Cyclopenta[b]pyridine, 4-chloro-6,7-dihydro-
4-Chloro-6,7-dihydro-5H-cyclopenta[b]pyridine 98%
5H-Cyclopenta[b]pyridine, 4-chloro-6,7-dihydro- ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
制備方法
90685-58-8
54664-55-0
以6,7-二氫-5H-環(huán)戊二烯并[b]吡啶1-氧化物(2.5g,18mmol)為原料,與磷酰氯(20mL,200mmol)混合。將反應(yīng)混合物在120℃下攪拌3小時(shí)。反應(yīng)完成后,通過(guò)減壓蒸餾除去過(guò)量的POCl3。將殘余物用80mL EtOAc稀釋?zhuān)⒂肗a2CO3溶液中和至pH 7-8。過(guò)濾后,水層用EtOAc萃取兩次(每次40mL)。合并有機(jī)萃取液,用無(wú)水Na2SO4干燥,過(guò)濾并減壓濃縮,得到4-氯-6,7-二氫-5H-環(huán)戊二烯并[b]吡啶(2.6g,收率93%)。LCMS分析:C8H9ClN(M + H)+的計(jì)算值:m/z = 154.2;實(shí)測(cè)值:154.3。
參考文獻(xiàn):
[1] Patent: US2014/200216, 2014, A1. Location in patent: Paragraph 0532; 0533
[2] Patent: US2014/200227, 2014, A1. Location in patent: Paragraph 0641; 0642
[3] Patent: WO2016/196244, 2016, A1. Location in patent: Page/Page column 195
[4] Patent: WO2009/19274, 2009, A1. Location in patent: Page/Page column 32
[5] Advanced Synthesis and Catalysis, 2007, vol. 349, # 14-15, p. 2345 - 2352