作　　者： ; ; ; ;

机构地区： 常州大学

出　　处： 《高校化学工程学报》 2017年第1期142-147,共6页

摘　　要： 以对二氯苯为起始原料,经过氧化氢氧化羟基化反应、二氧化碳羧基化反应,绿色合成了麦草畏中间体3,6-二氯水杨酸。重点研究了以V_2O_5为催化剂,过氧化氢为氧化剂,催化对二氯苯羟基化合成2,5-二氯苯酚的反应,考察了不同溶剂、主催化剂用量、助催化剂用量、氧化剂用量、反应温度、以及反应时间对羟基化反应收率的影响,确定了羟基化适宜反应条件为:n(对二氯苯):n(五氧化二钒):n(草酸):n(磷酸):n(过氧化氢)=0.1:0.00125:0.01:0.25:0.5,于30℃下反应10 h。2,5-二氯苯酚收率达39.3%,反应的总收率为31.3%。产物结构经过了1H-NMR,13C-NMR和GC-MS确定。所用方法原料廉价易得、反应条件温和、操作简便。 A green synthesis route of 3,6-dichlorosalicylic acid was reported via hydroxylation of 1,4-dichlorobenzene with hydrogen peroxide and followed by carboxylation with carbon dioxide. Thehydroxylation of 1,4-dichlorobenzene to prepare 2,5-dichlorophenol was studied using V2O5 as a catalyst and hydrogen peroxide as the oxidant. The effects of solvent, molar ratio of catalyst/oxidant to 1,4-dichlorobenzene,reaction temperature and reaction time on hydroxylation reaction yield were optimized. The optimizedhydroxylation conditions are n(C6H4Cl2):n(V2O5):n(C2H2O4):n(H3PO4):n(H2O2) = 0.1:0.00125:0.01:0.25:0.5 at30℃ for 10 h. 2,5-dichlorophenol is obtained with a yield of 39.3%. The total yield of 3,6-dichlorosalicylic acid is 31.3%. The chemical structure of the product was characterized by 1H-NMR, 13C-NMR and GC-MS. The proposed synthesis route is simple with mild reaction conditions and the raw materials are cheap and easy toobtain.

关 键 词： 对二氯苯 羟基化反应 二氯苯酚 二氯水杨酸

领　　域： [化学工程]