55368-42-8

基本信息
4-溴苯甲脒鹽酸鹽
4-溴芐脒鹽酸鹽 1G
4-溴苯甲脒鹽酸鹽水合物
4-溴芐脒鹽酸鹽(CAS號:55368-42-8)
4-BROMO-BENZAMIDINE HYDROCHLORIDE
Halogenobenzamidine hydrochloride
4-bromobenzimidamide hydrochloride
4-broMobenzaMidine hydrogen chloride
4-Bromo-benzamidine hydrochloride ,99%
4-Bromobenzamidine Hydrochloride Hydrate
amino(4-bromophenyl)methaniminium chloride
4-Bromobenzamidine Hydrochloride Hydrate>
4-broMobenzene-1-carboxiMidaMide hydrochloride
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

623-00-7

55368-42-8
以4-溴苯腈為原料合成4-溴苯脒鹽酸鹽的一般步驟如下:在-65℃條件下,將氯化氫氣體通入含有4-溴芐腈(18.2g)的氯仿(300mL)和乙醇(100mL)混合溶液中,持續(xù)35分鐘。隨后,將反應(yīng)體系緩慢升溫至室溫,并在該溫度下持續(xù)攪拌過夜。反應(yīng)完成后,通過真空蒸發(fā)去除溶劑,得到的殘余物用乙醇(400mL)重新溶解。向此溶液中加入碳酸銨(48.0g),反應(yīng)混合物在室溫下攪拌20小時(shí)。反應(yīng)結(jié)束后,加入水(300mL),并通過真空濃縮去除乙醇。過濾收集生成的沉淀,用水洗滌后,進(jìn)行真空干燥,得到目標(biāo)產(chǎn)物4-溴苯脒鹽酸鹽(22.9g,收率97%),為白色固體。產(chǎn)物經(jīng)1H NMR(DMSO-d6)檢測,顯示δ2.55-4.60(2H,寬峰),6.30-8.90(6H,多重峰);FAB-MS檢測顯示m/z 199,201 [(M + H)+]。
參考文獻(xiàn):
[1] Bioorganic and Medicinal Chemistry, 2012, vol. 20, # 7, p. 2369 - 2375
[2] Bioorganic and Medicinal Chemistry, 2017, vol. 25, # 23, p. 6218 - 6223
[3] Magnetic Resonance in Chemistry, 1987, vol. 25, p. 923 - 927
[4] Physical Chemistry Chemical Physics, 2004, vol. 6, # 4, p. 756 - 765
[5] Tetrahedron Letters, 2018, vol. 59, # 4, p. 361 - 364