20986-40-7
20986-40-7 結(jié)構(gòu)式
基本信息
5-溴煙酸乙脂
5-BROMONICOTINIC ACID ETHYL ESTER
AURORA KA-3028
ETHYL 5-BROMO-3-PYRIDINECARBOXYLATE
ETHYL 5-BROMONICOTINATE
ETHYL 5-BROMOPYRIDINE-3-CARBOXYLATE
TIMTEC-BB SBB005820
Ethyl 5-bromopyridine-3-carboxylic acid
Ethyl-5-Bromonicotinate98%
5-Bromonicotinicacidethylester~Ethyl5-bromopyridine-3-carboxylate
5-Bromo Nitinic Acid Ethyl Ester
5-Bromonicotinic acid ethyl ester 97%
Ethyl 5-bromonicotinate 97%
5-BROMONICOTIC ACID ETHYL ESTER
Ethyl 5-Bromonicotinic acid ethyl ester
5-Bromopyridine-3-carboxylic acid ethyl ester
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法
20826-04-4
64-17-5
20986-40-7
a) 5-溴煙酸乙酯的合成：在攪拌下，將濃H2SO4（9.0 mL）緩慢滴加至5-溴煙酸（3.00 g，14.9 mmol）的乙醇（30.0 mL）懸浮液中，滴加時(shí)間控制在5分鐘內(nèi)，直至形成澄清溶液。隨后，將反應(yīng)混合物加熱回流22小時(shí)。反應(yīng)完成后，冷卻至室溫，用水（30 mL）淬滅反應(yīng)，然后用二氯甲烷（75 mL）萃取。有機(jī)層依次用10% Na2CO3溶液（20 mL）和水（20 mL）洗滌，無(wú)水MgSO4干燥，經(jīng)燒結(jié)玻璃漏斗過(guò)濾后濃縮，得到白色固體5-溴煙酸乙酯2.8 g，收率82%。產(chǎn)物結(jié)構(gòu)經(jīng)1H NMR（CDCl3）確認(rèn)：δ 9.13（d, J = 1.7 Hz, 1H），8.84（d, J = 2.2 Hz, 1H），8.42（m, J = 2.2, 1.7 Hz, 2H），4.40（q, J = 7.1 Hz, 2H），1.43（t, J = 7.1 Hz, 3H）。
參考文獻(xiàn)：
[1] Patent: WO2008/151073, 2008, A1. Location in patent: Page/Page column 39-40; 44
[2] Journal of Organic Chemistry, 2001, vol. 66, # 12, p. 4115 - 4121
[3] Patent: US2016/375131, 2016, A1. Location in patent: Paragraph 0080
[4] ACS Combinatorial Science, 2017, vol. 19, # 5, p. 286 - 298
[5] Organic Preparations and Procedures International, 1992, vol. 24, # 2, p. 143 - 146