林产化学与工业
林產化學與工業
림산화학여공업
CHEMISTRY AND INDUSTRY OF FOREST PRODUCTS
2014年
2期
103-107
,共5页
冯虹钧%杨久芳%高飞飞%罗金岳%陆强%徐徐
馮虹鈞%楊久芳%高飛飛%囉金嶽%陸彊%徐徐
풍홍균%양구방%고비비%라금악%륙강%서서
萘二酚%萘二醌%芳构化%月桂烯
萘二酚%萘二醌%芳構化%月桂烯
내이분%내이곤%방구화%월계희
hydronaphthoquinone%morkit%aromatization%myrcene
以对苯醌与月桂烯为起始原料,合成了萘二酚衍生物,经芳构化制备了产物萘二醌衍生物。采用GC-MS、红外光谱和1H NMR等手段对产物进行了表征,确证产物为6-(4-甲基-3-戊烯基)-1,4-萘二醌。利用单因素试验系统考察了催化剂种类、催化剂用量、反应温度、反应时间和溶剂种类对产物得率的影响,得到适宜的工艺条件是:萘二酚用量0.02 mol,催化剂为活性二氧化锰,用量0.05 mol,溶剂为乙酸乙酯,反应温度80℃,反应时间22 h,此条件下目标产物得率达到88.6%。活性二氧化锰催化剂可重复使用4次,得率下降不明显。
以對苯醌與月桂烯為起始原料,閤成瞭萘二酚衍生物,經芳構化製備瞭產物萘二醌衍生物。採用GC-MS、紅外光譜和1H NMR等手段對產物進行瞭錶徵,確證產物為6-(4-甲基-3-戊烯基)-1,4-萘二醌。利用單因素試驗繫統攷察瞭催化劑種類、催化劑用量、反應溫度、反應時間和溶劑種類對產物得率的影響,得到適宜的工藝條件是:萘二酚用量0.02 mol,催化劑為活性二氧化錳,用量0.05 mol,溶劑為乙痠乙酯,反應溫度80℃,反應時間22 h,此條件下目標產物得率達到88.6%。活性二氧化錳催化劑可重複使用4次,得率下降不明顯。
이대분곤여월계희위기시원료,합성료내이분연생물,경방구화제비료산물내이곤연생물。채용GC-MS、홍외광보화1H NMR등수단대산물진행료표정,학증산물위6-(4-갑기-3-무희기)-1,4-내이곤。이용단인소시험계통고찰료최화제충류、최화제용량、반응온도、반응시간화용제충류대산물득솔적영향,득도괄의적공예조건시:내이분용량0.02 mol,최화제위활성이양화맹,용량0.05 mol,용제위을산을지,반응온도80℃,반응시간22 h,차조건하목표산물득솔체도88.6%。활성이양화맹최화제가중복사용4차,득솔하강불명현。
The myrcene and 1, 4-benzoquinone are used as raw materials to synthesize naphthalene catechol derivatives of naphthalene-1,4-diol. Further the naphthalene catechol derivatives of naphthalene-1,4-dione is synthesized by aromatization. The structure of the product is identified as 6-( 4-methylpent-3-enyl ) naphthalene-1, 4-dione by GC-MS, the FT-IR, 1H NMR characterization. The synthesis conditions from hydronaphthoquinone to morkit were investigated. The experimental parameters such as different type of catalysts, catalyst amount, reaction solvent, reaction temperature and reaction time have been investigated systematically with single-factor experimentation to obtain maximum yield. It is concluded that the fittest catalyst is manganese(IV) oxide, while the dosage of naphthalene-1,4-diol and catalyst is 0. 02 mol and 0. 05 mol, respectively. Acetic ester is chosen as solvent and the reaction temperature is 80 ℃, reaction time is 22 h. Under this condition, the yield of product reached 88.6%. Manganese( IV) oxide catalyst can be reused four times, while the yield decline is not obvious.