188187-03-3

基本信息
2-(BroMoMethyl)-3-chloro-benzoic acid Methyl ester
Benzoic acid, 2-(bromomethyl)-3-chloro-, methyl ester
物理化學(xué)性質(zhì)
常見問題列表

99586-84-2

188187-03-3
以3-氯-2-甲基苯甲酸甲酯(1g,5.42mmol)為原料,將其與四氯化碳(13.3ml)、N-溴代琥珀酰亞胺(1.06g,5.96mmol)及過氧化苯甲酰(3.5mg,0.0108mmol)混合形成懸浮液。在氮氣保護下,將反應(yīng)混合物置于90℃的油浴中加熱。反應(yīng)進行3小時45分鐘后,停止加熱。反應(yīng)液依次用水、乙酸乙酯和飽和碳酸氫鈉水溶液稀釋。分離有機層,用飽和碳酸氫鈉水溶液洗滌,無水硫酸鎂干燥,過濾后濃縮,得到目標產(chǎn)物2-溴甲基-3-氯-苯甲酸甲酯(1.43g,產(chǎn)率:100%)。產(chǎn)物經(jīng)1H-NMR(400MHz,CDCl3)表征,化學(xué)位移δppm分別為:4.00(3H,s),5.12(2H,s),7.32(1H,t,J = 8 Hz),7.58(1H,dd,J = 2,8 Hz),7.86(1H,dd,J = 2,8 Hz)。
參考文獻:
[1] Patent: US2013/65925, 2013, A1. Location in patent: Paragraph 0338; 0339
[2] Patent: EP2757103, 2014, A1. Location in patent: Paragraph 0215
[3] Patent: US5958968, 1999, A
[4] Patent: WO2004/58717, 2004, A1. Location in patent: Page 77
[5] Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 1, p. 360 - 365