硒催化3-氯-4-甲基硝基苯羰基化合成绿麦隆

Selenium-catalyzed Carbonylation of 3-chloro-4-methyl-nitrobenzene to Chlortoluron Herbicide

以硒为催化剂、有机胺为助催化剂、3-氯-4-甲基硝基苯和二甲胺为反应底物,经高选择性氧化还原羰基化一步合成绿麦隆。在丙酮和甲苯溶剂中,155℃、4.0MPa时反应4h,单程最高收率可达62%,选择性为99%以上,催化剂及其催化体系均可以循环使用,循环收率的平均值可达75%。

The oxidativc-rcductive carbonylation of dimethyamine and 3-chloro-4-methyl-nitrobvnzene catalyzed by selenium and organic base as cocatalyst to yield chlortoluron herbicide has been studied. On the condition of 155℃, 4.0 MPa and 4 h, the yield is reached 62%, the selectivity of chlortoluron is above 99% in acetone/toluene solvent. The Se catalyst and chlortoluron are easily separated, both catalyst and catalytic system may be recycled in organic solvent. The average yields recycled of chlortoluron is reached above 75%.