广州化工
廣州化工
엄주화공
GUANGZHOU CHEMICAL INDUSTRY AND TECHNOLOGY
2012年
9期
77-78
,共2页
蔡亚祥%位军辉%徐建康%朱国良%车大庆
蔡亞祥%位軍輝%徐建康%硃國良%車大慶
채아상%위군휘%서건강%주국량%차대경
2-氨基-4-异丙基-5-溴苯甲酸%间异丙基苯胺%环合%溴化%氧化%合成
2-氨基-4-異丙基-5-溴苯甲痠%間異丙基苯胺%環閤%溴化%氧化%閤成
2-안기-4-이병기-5-추분갑산%간이병기분알%배합%추화%양화%합성
2 - amino - 4 - isopropyl - 5 - bromobenzoic acid%m - isopropylaniline%cyclization%bromination%oxi- dation%synthesis
以间异丙基苯胺为起始原料,与水合氯醛、盐酸羟胺反应后,经Sandmeyer法环合、溴化、氧化得到目标化合物2-氨基-5-溴-4-异丙基苯甲酸。目标化合物的结构经红外光谱、^1HNMR和Ms确证。该合成方法具有原料易得,合成路线短,操作简单,生产成本低廉的优点,总收率由文献报道的28%提高到39%,更适合工业化生产。
以間異丙基苯胺為起始原料,與水閤氯醛、鹽痠羥胺反應後,經Sandmeyer法環閤、溴化、氧化得到目標化閤物2-氨基-5-溴-4-異丙基苯甲痠。目標化閤物的結構經紅外光譜、^1HNMR和Ms確證。該閤成方法具有原料易得,閤成路線短,操作簡單,生產成本低廉的優點,總收率由文獻報道的28%提高到39%,更適閤工業化生產。
이간이병기분알위기시원료,여수합록철、염산간알반응후,경Sandmeyer법배합、추화、양화득도목표화합물2-안기-5-추-4-이병기분갑산。목표화합물적결구경홍외광보、^1HNMR화Ms학증。해합성방법구유원료역득,합성로선단,조작간단,생산성본저렴적우점,총수솔유문헌보도적28%제고도39%,경괄합공업화생산。
The target compound of 2 -amino -4 -isopropyl -5 -bromobenzoic acid was synthesized from misoprop- ylaniline by reaction with chlora hydrate/hydroxylamine hydrochloride and then by cyclization of Sandmeyer method, bromination and oxidation, the structure of the target compound was confirmed by IR, 1H - NMR and MS. The synthetic procedure was suitable for industrial production for the advantage of avaible materials, shorter routes, convenient operation and lower cost, the overall yield was improved from the reported 28% to 39%.