34547-28-9

基本信息
4-氟苯乙酰肼
對(duì)氟苯乙酸酰肼
2-(4-氟苯基)乙酰肼
P-FLUOROPHENYLACETYL HYDRAZINE
4-flourophenyl acetic hydrazide
4-FLUOROPHENYL ACETIC HYDRAZIDE
Of acetyl hydrazine fluorophenyl
4-Fluorophenylacetic acid hydrazide
Benzeneacetic acid, 4-fluoro-, hydrazide
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

459-04-1

34547-28-9
以4-氟苯乙酰氯為原料合成2-(4-氟苯基)乙酰肼的一般步驟如下:在0℃下,將肼(4.5M,144mmol)的二氯甲烷(50mL)溶液緩慢滴加至(4-氟苯基)乙酰氯(1.0g,5.8mmol)的二氯甲烷溶液中。反應(yīng)混合物在0℃下攪拌40分鐘。隨后,加入水終止反應(yīng)。分離有機(jī)層和水層,水層用二氯甲烷萃取。合并所有有機(jī)相,用無水硫酸鈉干燥。過濾除去干燥劑,濾液經(jīng)減壓濃縮后,通過快速柱色譜法純化(洗脫梯度:5%甲醇-二氯甲烷),得到2-(4-氟苯基)乙酰肼(673mg,收率69%)為白色固體。產(chǎn)物經(jīng)1H NMR(DMSO-D6)表征:δ 9.18(寬峰,1H),7.26(dd,J = 8.4, 5.7 Hz,2H),7.09(t,J = 8.4 Hz,2H),4.21(寬峰,2H),3.31(s,2H);質(zhì)譜(MS)顯示m/z 169([M + H]+)。
參考文獻(xiàn):
[1] Medicinal Chemistry, 2014, vol. 10, # 8, p. 810 - 823
[2] Patent: WO2004/101512, 2004, A2. Location in patent: Page 55
[3] Patent: WO2007/50510, 2007, A2. Location in patent: Page/Page column 38
[4] Patent: WO2011/46873, 2011, A1. Location in patent: Page/Page column 29
[5] Patent: WO2011/120153, 2011, A1