25081-39-4

基本信息
3,5-二甲基苯甲酸甲酯,98%
METHYL 3,5-DIMETHYLBENZOATE
3,5-Dimethylbenzoic acid methyl
Methyl 3,5-dimethylbenzoate 98%
3,5-DIMETHYLBENZOIC ACID METHYL ESTER
Benzoic acid, 3,5-dimethyl-, methyl ester
物理化學(xué)性質(zhì)
制備方法

499-06-9

67-56-1

25081-39-4
以3,5-二甲基苯甲酸(1.0g,0.0081mol)和甲醇(3mL)為原料,在高壓釜中加入溴苯(0.125g,0.0081mol)和10%鈀碳(50%濕,0.2g)。用氮?dú)猓?-2巴)對高壓釜進(jìn)行加壓,隨后加入氫氣(1-2巴),并調(diào)整至所需的氫氣壓力(5-6巴)。將反應(yīng)混合物加熱至55-60℃,并在300轉(zhuǎn)/分鐘下攪拌4小時(shí)。反應(yīng)完成后,通過硅藻土床過濾以去除催化劑。向?yàn)V液中加入水(30mL),用乙酸異丙酯(2×15mL)萃取反應(yīng)混合物。合并有機(jī)層,用5%碳酸氫鈉水溶液(2×15mL)洗滌,無水Na2SO4干燥后過濾。最后,通過真空蒸發(fā)濾液,得到3,5-二甲基苯甲酸甲酯產(chǎn)物。
參考文獻(xiàn):
[1] Helvetica Chimica Acta, 1996, vol. 79, # 7, p. 1967 - 1979
[2] Journal of Organic Chemistry, 2006, vol. 71, # 19, p. 7205 - 7213
[3] Monatshefte fur Chemie, 1996, vol. 127, # 2, p. 185 - 200
[4] European Journal of Organic Chemistry, 2009, # 26, p. 4480 - 4485
[5] Tetrahedron Letters, 2013, vol. 54, # 42, p. 5690 - 5694