1353100-91-0

基本信息
3-溴-1-H-吡唑-4-羧酸乙酯
3-Bromo-4-(ethoxycarbonyl)-1H-pyrazole
1-H-pyrazole-4-carboxylic acid,3-broMo,ethyl ester
3-broMo-1-H-pyrazole-4-carboxylic acid ethyl ester
物理化學(xué)性質(zhì)
常見(jiàn)問(wèn)題列表

6994-25-8

1353100-91-0
以3-氨基-4-乙氧羰基吡唑?yàn)樵虾铣?-溴吡唑-4-甲酸乙酯的一般步驟如下:在0℃下,向3-氨基-1H-吡唑-4-羧酸乙酯(5.0g,32mmol)和溴化銅(II)(7.2g,32mmol)的乙腈(65mL)溶液中緩慢加入異戊基亞硝酸鹽(12mL,86mmol)。將反應(yīng)混合物加熱至50℃并攪拌過(guò)夜。反應(yīng)完成后,將混合物冷卻至室溫,并用1N鹽酸水溶液(150mL)淬滅反應(yīng)。用乙酸乙酯(3×100mL)萃取混合物。合并有機(jī)相,用水洗滌,用無(wú)水硫酸鈉干燥,過(guò)濾并濃縮,得到3-溴吡唑-4-甲酸乙酯,為棕色油狀物,在真空下部分固化過(guò)夜(7.1g,100%)。產(chǎn)物經(jīng)1H NMR(400MHz,CDCl3)表征:δ 9.78(br.s,1H),8.10(br.s,1H),4.33(q,J = 7.22Hz,2H),1.36(m,3H)。
參考文獻(xiàn):
[1] Patent: US2012/108619, 2012, A1. Location in patent: Page/Page column 26
[2] Patent: WO2012/9009, 2012, A2. Location in patent: Page/Page column 56
[3] Patent: WO2012/8999, 2012, A2. Location in patent: Page/Page column 75
[4] Journal of Organic Chemistry, 2012, vol. 77, # 22, p. 10050 - 10057
[5] Patent: WO2014/188211, 2014, A1. Location in patent: Page/Page column 78