18362-30-6

基本信息
2-氯-6-羥基苯甲醛
2-氯-6-羥基苯甲醛,6-氯水楊醛
6-氯水楊醛(2-氯-6-羥基苯甲醛)
6-chloro salicyaldehyde
2-CHLORO-6-HYDROXYBENZALDEHYDE
2-chloro-6-hydroxy-benzaldehyd
6-Chloro-2-hydroxybenzaldehyde
Benzaldehyde, 2-chloro-6-hydroxy-
6-Chlorosalicylaldehyde, 3-Chloro-2-formylphenol
6-chloro salicyaldehyde 2-chloro-6-hydroxybenzaldehyde
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

387-45-1

18362-30-6
以2-氯-6-氟-苯甲醛為原料合成6-氯水楊醛的一般步驟如下:在0℃條件下,將氫氧化鉀(10g)緩慢加入至攪拌中的2-氯-6-氟-苯甲醛(14.0g,88.3mmol)的二甲基亞砜(20mL)溶液中。隨后,將反應(yīng)混合物逐漸升溫至室溫,并持續(xù)攪拌18小時(shí)。反應(yīng)完成后,用100mL水稀釋反應(yīng)混合物,并用濃鹽酸調(diào)節(jié)pH至2。通過過濾收集沉淀物,先后用100mL水洗滌兩次,再用無水硫酸鈉干燥,得到粗產(chǎn)物,該產(chǎn)物無需進(jìn)一步純化即可用于后續(xù)反應(yīng)。最終產(chǎn)量為8.5克,收率為62%。產(chǎn)物結(jié)構(gòu)經(jīng)1H NMR(400MHz,CDCl3)確認(rèn),δppm6.65-7.02(m,2H),7.39-7.47(m,1H),10.41(s,1H),11.95(s,1H)。
參考文獻(xiàn):
[1] European Journal of Organic Chemistry, 2018, vol. 2018, # 25, p. 3348 - 3351
[2] Patent: WO2012/87229, 2012, A1. Location in patent: Page/Page column 14
[3] Patent: US2008/171754, 2008, A1. Location in patent: Page/Page column 89
[4] Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1993, # 12, p. 1345 - 1358
[5] Zeitschrift fuer Naturforschung, Teil B: Anorganische Chemie, Organische Chemie, Biochemie, Biophysik, Biologie, 1972, vol. 27, p. 663 - 674