应用化学
應用化學
응용화학
CHINESE JOURNAL OF APPLIED CHEMISTRY
2009年
11期
1374-1376
,共3页
陈韶蕊%马吉海%周雪琴%刘东志
陳韶蕊%馬吉海%週雪琴%劉東誌
진소예%마길해%주설금%류동지
十二烷二酸%偶联缩合%环十二二酮
十二烷二痠%偶聯縮閤%環十二二酮
십이완이산%우련축합%배십이이동
dodecanedioic acid%acyloin condensation%cyclododecandione
以十二烷二酸(1)为原料,与甲醇酯化生成十二烷二酸二甲酯(2),收率为86.5%.化合物2经偶联缩合得1,2-二三甲基硅氧基环十二烯(3),收率为63.1%. 利用溴氧化化合物3得到1,2-环十二二酮(4)淡黄色晶体,收率79%,全过程收率达43.1%,是合成1,2-二酮的新方法. 目标化合物结构经红外光谱、核磁共振氢谱和碳谱表征确认.
以十二烷二痠(1)為原料,與甲醇酯化生成十二烷二痠二甲酯(2),收率為86.5%.化閤物2經偶聯縮閤得1,2-二三甲基硅氧基環十二烯(3),收率為63.1%. 利用溴氧化化閤物3得到1,2-環十二二酮(4)淡黃色晶體,收率79%,全過程收率達43.1%,是閤成1,2-二酮的新方法. 目標化閤物結構經紅外光譜、覈磁共振氫譜和碳譜錶徵確認.
이십이완이산(1)위원료,여갑순지화생성십이완이산이갑지(2),수솔위86.5%.화합물2경우련축합득1,2-이삼갑기규양기배십이희(3),수솔위63.1%. 이용추양화화합물3득도1,2-배십이이동(4)담황색정체,수솔79%,전과정수솔체43.1%,시합성1,2-이동적신방법. 목표화합물결구경홍외광보、핵자공진경보화탄보표정학인.
1,2-Cyclododecandione (4) was synthesized from dodecanedioic acid via esterification, acyloin condensation, oxidation in an overall yield of 43. 1 %. Reaction of dodecanedioic acid with methanol gave dodecanedioic acid dimethyl ester(2) with a yield of 86. 5%. Compound 3 was obtained from compound 2 through acyloin condensation and the yield reached up to 63. 1% , which was oxidized to compound 4 by bromine water as the oxidation reagent with a yield of 79%. The target compound was a light yellow crystal and was characterized by means of IR, ~1H NMR and ~(I3)C NMR.