Barbosa Sandro L, Lima Camila D, Almeida Melina A R, Mourão Larissa S, Ottone Myrlene, Nelson David L, Klein Stanlei I, Zanatta Lucas D, Clososki Giuliano C, Caires Franco J, Nassar Eduardo J, Hurtado Gabriela R
Department of Pharmacy, Universidade Federal dos Vales do Jequitinhonha e Mucuri - UFVJM, Campus JK, Rodovia MGT 367 - Km 583, n 5000, Alto da Jacuba, CEP 39100-000 Diamantina, MG, Brazil.
Department of General and Inorganic Chemistry, Institute of Chemistry, São Paulo State University - Unesp, R. Prof. Francisco Degni, n 55, Quitandinha, CEP 14800-060 Araraquara, SP, Brazil.
Heliyon. 2018 Mar 16;4(3):e00571. doi: 10.1016/j.heliyon.2018.e00571. eCollection 2018 Mar.
Two solvent free methods of a one-to-one alcohol/acid mol ratio synthesis of benzyl esters of the formic, acetic, benzoic, salicylic, nicotinic, and oxalic acids are described. The stoichiometric reactions used 1.5 mol ratio solid NbCl as the reagent and required from two to three hours for completion at room temperature; for the catalytic processes, NbCl was grafted directly, at room temperature, onto a silica gel of specific area of 507 mg, produced from construction sand and sodium carbonate, forming a 5.4% Nb w/w SiO-Nb gel with a specific area of 412 mg. At 10% w/w catalyst/alcohol ratio, this SiO-Nb catalyst gave similarly very good yields but required from 6 to 9 hours at the reflux temperature of the slurry. The catalyst could be re-used three times.
描述了两种无溶剂方法,用于以1:1的醇/酸摩尔比合成甲酸、乙酸、苯甲酸、水杨酸、烟酸和草酸的苄酯。化学计量反应使用1.5摩尔比的固体NbCl作为试剂,在室温下完成反应需要两到三个小时;对于催化过程,在室温下将NbCl直接接枝到由建筑砂和碳酸钠制备的比表面积为507mg的硅胶上,形成比表面积为412mg的5.4%Nb w/w SiO-Nb凝胶。在10%w/w的催化剂/醇比例下,这种SiO-Nb催化剂同样能给出非常好的产率,但在淤浆回流温度下需要6到9小时。该催化剂可以重复使用三次。