16740-73-1

基本信息
5-溴-2-甲氧基乙?;?BR>1-(5-溴-2-甲氧基苯基)-乙酮
1-(5-溴-2-甲氧基苯基)乙-1-酮
1-(5-Bromo-2-methoxyphenyl)ethan-1-one
JR-8526, 1-(5-Bromo-2-methoxyphenyl)ethanone, 97%
常見問題列表

579-74-8

16740-73-1
以2'-甲氧基苯乙酮為原料合成1-(5-溴-2-甲氧基苯基)-乙酮的一般步驟:向反應管中加入N-溴代琥珀酰亞胺(NBS,1.5當量,0.3 mmol)、催化劑(10 mol%,0.02 mmol)及乙腈(CH3CN,1.0 mL),隨后加入2'-甲氧基苯乙酮(0.2 mmol)。反應混合物在室溫下避光攪拌12小時。反應完成后,用飽和硫代硫酸鈉(Na2S2O3)水溶液(2 mL)淬滅反應。用乙酸乙酯(3.5 mL)萃取反應混合物。合并有機相,用鹽水(10 mL)洗滌,無水硫酸鈉(Na2SO4)干燥,并通過硅藻土墊過濾。濾液減壓濃縮,殘留物通過硅膠柱快速色譜純化,使用石油醚/二氯甲烷(5:1)作為洗脫劑,得到目標產物1-(5-溴-2-甲氧基苯基)-乙酮。
參考文獻:
[1] Tetrahedron, 2017, vol. 73, # 50, p. 7105 - 7114
[2] Tetrahedron Letters, 2006, vol. 47, # 27, p. 4707 - 4710
[3] Patent: US9138427, 2015, B2. Location in patent: Page/Page column 312-313
[4] Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1987, p. 1423 - 1428
[5] Synthesis (Germany), 2013, vol. 45, # 11, p. 1497 - 1504