2,4-双(辛基硫亚甲基)-6-甲基苯酚的合成

Synthesis of 2,4-Bis(n-Octylthiomethyl)-6-Methylphenol

以邻甲酚、正辛硫醇和多聚甲醛为原料,以六次甲基四胺为催化剂、N,N-二甲基甲酰胺(DMF)为溶剂,在氮气气氛中采用一步法合成了2,4-双(辛基硫亚甲基)-6-甲基苯酚。采用4因素3水平正交实验研究了原料配比、反应时间、反应温度和催化剂用量等因素对合成反应的影响,并通过单因素实验得到了最佳反应条件,即邻甲酚75 mmol、n(邻甲酚):n(正辛硫醇):n(多聚甲醛)=1.00:2.10:4.20、催化剂用量7mmol、DMF 22mL、反应温度110℃、反应时间9h;在此条件下,2,4-双(辛基硫亚甲基)-6-甲基苯酚收率为93.46%。产品经IR表征和元素分析确证为目标化合物。

2, 4-Bis（n-octylthiomethyl）-6-methylphenol was synthesized from o-cresol, n-octanethiol and paraformaldehyde with hexamethylenetetramine as the catalyst and N, N-dimethylformamide（DMF） as the solvent by an one-step method under nitrogen protection. The effects of raw material ratio, reaction time, reaction temperature and catalyst dosage on the synthesis were investigated by orthogonal experiments. The optimum reaction conditions were obtained by single-factor experiments. Under the optimum reaction conditions of o-cresol dosage 75 mmol, n（o-cresol） ： n（n-octanethiol） ： n（paraformaldehyde） 1.00 ： 2.10 ： 4.20, catalyst dosage 7 mmol, DMF dosage 22 mL, reaction temperature 110 ℃ and reaction time 9 h, the yield of 2, 4-bis- （n-octylthiomethyl）-6-methylphenol reached 93.46%. The product was verified by means of IR and elemental analysis.