24190-77-0

基本信息
3-氯-4-乙酰氨基水楊酸甲酯
3-氯-4-乙酰胺基水楊酸甲酯
2-羥基-4-乙酰氨基-5-氯苯甲酸甲酯
4-乙酰氨基-5-氯-2-羥基苯甲酸甲酯
5-氯-2-羥基-4-乙酰氨基苯甲酸甲酯
4-乙酰氨基-5-氯-2-羥基苯甲酸甲酯 100G
Methyl 4-acetamido-5-chlorosalicylate
4-acetylamino-5-chloro-2-methoxybenzoate
4-acetylaMino-5-chloro-2-hydroxybenzoate
Methyl 5-chloro-4-acetaMido-2-hydroxybenzoate
Methyl 2-hydroxy-4-acetamido-5-chlorobenzoate
methyl 4-acetamido-2-hydroxy-5-chlorobenzoate
Methyl 4-acetylaMino-5-chloro-2-hdroxybenzoate
METHYL 4-ACETYLAMINO-5-CHLORO-2-HYDROXYBENZOATE
4-Acetamido-5-chloro-2-hydroxybenzoic acid methyl ester
物理化學(xué)性質(zhì)
常見問題列表

4093-28-1

24190-77-0
以4-乙酰氨基-2-羥基苯甲酸甲酯(61.4克,294.0毫摩爾)為原料,在二氯乙烷(1.2升)中攪拌溶解,隨后加入N-氯代琥珀酰亞胺(58.8克,441毫摩爾)。將反應(yīng)混合物加熱回流3小時。反應(yīng)完成后,通過減壓蒸餾去除揮發(fā)性溶劑。向殘余物中加入水(1.0升)以沉淀固體產(chǎn)物,經(jīng)過濾收集。粗產(chǎn)物用甲醇與二氯甲烷的混合溶劑(體積比1:9)溶解,并用飽和鹽水洗滌。有機層經(jīng)無水硫酸鈉干燥后,減壓濃縮,得到4-乙酰氨基-5-氯-2-羥基苯甲酸甲酯(67.7克),產(chǎn)率為94.6%。產(chǎn)物結(jié)構(gòu)經(jīng)核磁共振氫譜(DMSO-d6)確認:δ10.49(寬單峰,1H),9.47(單峰,1H),7.75(單峰,1H),7.72(單峰,1H),3.85(單峰,3H),2.16(單峰,3H);質(zhì)譜分析顯示分子離子峰(m/z)為244和246(M+H)+。
參考文獻:
[1] Patent: WO2013/42135, 2013, A1. Location in patent: Page/Page column 11
[2] Patent: US2014/187581, 2014, A1. Location in patent: Paragraph 0098-0100
[3] Patent: WO2016/128990, 2016, A1. Location in patent: Page/Page column 26-27
[4] Bioorganic and Medicinal Chemistry Letters, 1996, vol. 6, # 22, p. 2657 - 2662
[5] Patent: CN107337658, 2017, A. Location in patent: Paragraph 0043; 0044