37687-57-3

基本信息
2-氯代異香蘭素 1G
2-氯-3-羥基對(duì)茴香醛
2-氯-3-羥基-4-甲氧基苯甲醛
chloroisovanilin
Chloroisovaniline
2-CHLOROISOVANILLIN
TIMTEC-BB SBB003704
2-CHLORO-3-HYDROXY-P-ANISALDEHYDE
2-CHLORO-3-HYDROXY-4-METHOXYBENZALDEHYDE
Benzaldehyde, 2-chloro-3-hydroxy-4-methoxy-
2-Chloro-3-hydroxy-4-methoxybenzaldehyde 97%
2-Chloro-3-hydroxy-p-anisaldehyde, 2-Chloroisovanillin
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
常見(jiàn)問(wèn)題列表

621-59-0

37687-57-3
步驟1 2-氯-3-羥基-4-甲氧基苯甲醛的合成:將41.2 g(0.271 mol)異香草醛在加熱條件下溶解于160 mL 90%的乙酸中。在35℃至40℃條件下,緩慢滴加29.41 g叔丁基次氯酸鹽(t-BuOCl)至上述溶液中。反應(yīng)混合物在室溫下攪拌3小時(shí),隨后加入200 mL乙醚。將混合物靜置過(guò)夜,通過(guò)過(guò)濾分離析出的晶體,并用乙醚洗滌。粗產(chǎn)物(42.0 g)通過(guò)乙腈重結(jié)晶純化,得到35 g 2-氯-3-羥基-4-甲氧基苯甲醛,收率69%。產(chǎn)物熔點(diǎn)為203~205℃。核磁共振氫譜(90 MHz,DMSO-d6)δ:3.94(3H,s,OCH3),7.10(1H,d,Ar-H),7.42(1H,d,Ar-H),9.84(1H,s,CHO),10.16(1H,s,OH)。
參考文獻(xiàn):
[1] Journal of Medicinal Chemistry, 1986, vol. 29, # 11, p. 2315 - 2325
[2] Organic Process Research and Development, 2001, vol. 5, # 1, p. 45 - 49
[3] Synlett, 2014, vol. 25, # 20, p. 2891 - 2894
[4] Journal of Organic Chemistry, 2012, vol. 77, # 2, p. 977 - 984
[5] Journal of Heterocyclic Chemistry, 1986, vol. 23, # 6, p. 1805 - 1814