20776-63-0

基本信息
2-AMINO-4,6-DICHLOROBENZOIC ACID
Benzoic acid, 2-amino-4,6-dichloro-
2-AMINO-4,6-DICHLOROBENZOIC ACID FOR SYN
2-Amino-4,6-dichlorobenzoic acid for synthesis
2-AMINO-4,6-DICHLOROBENZOIC ACID ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

18711-15-4

20776-63-0
以4,6-二氯二氫吲哚-2,3-二酮為原料合成2-氨基-4,6-二氯苯甲酸的一般步驟: 3)中間體I-3的制備; 在室溫下,將上述分離實(shí)施例I(2)制備的中間體I-2(5.0g,23.1mmol)溶于75mL 1N NaOH(aq)中,分批加入過氧化氫(28%v/v,10mL)。反應(yīng)混合物攪拌2小時后過濾,去除不溶的深棕色固體。隨后,將濾液小心地用鹽酸酸化至pH 2。收集形成的黃色沉淀,用水洗滌,并在真空下干燥。通過從苯中重結(jié)晶得到目標(biāo)化合物2-氨基-4,6-二氯苯甲酸(3.90g,產(chǎn)率82%),為象牙色固體。 TLC Rf = 0.1(EtOAc:正己烷=1:1); 熔點(diǎn)188-189°C; 1H NMR(DMSO-d6)δ6.76(d,J=1.9Hz,1H,ArH),6.85(d,J=1.9Hz,1H,ArH); MS(EI)m/e 206 [M+],162 [M+-CO2]。
參考文獻(xiàn):
[1] Patent: US2006/84676, 2006, A1. Location in patent: Page/Page column 7
[2] Patent: EP1650190, 2006, A1. Location in patent: Page/Page column 10
[3] Patent: WO2008/4716, 2008, A1. Location in patent: Page/Page column 25-26
[4] Bioorganic and Medicinal Chemistry Letters, 2008, vol. 18, # 2, p. 738 - 743
[5] Patent: US2009/203708, 2009, A1. Location in patent: Page/Page column 8