摘要
以国产Ｄｏｏ／ＣＣ树脂为催化剂，将假性甲基紫罗兰酮环化为甲基紫罗兰酮。考察了溶剂、Ｄｏｏ／ＣＣ用量、反应温度、反应时间等因素对环化产率的影响，得出优化的反应条件为：溶剂为二氯甲烷，Ｄｏｏ／ＣＣ用量为假性甲基紫罗兰酮质量的１５倍，反应温度为体系的回流温度（４５℃），反应时间为４ｈ。按此条件进行平行实验，平均产率７９９％，沸点９０～１００℃／２６７～４００Ｐａ，ｎ２０Ｄ＝１５０００～１５０２０，甲基紫罗兰酮含量９１８％。考察了催化剂的活性，Ｄｏｏ／ＣＣ树脂连续使用７次，环化平均产率为８０６％。
In cyclization of pseudmethylionone macroreticular resin Doo/CC as catalyst was used. The factors of effecting the cyclization were studied,and optimum condition of cyclization, in the dichloromethane for 4h at 45℃,was obtained and quantity of cyclization agent was 150% of pseudmethylionone. The yield of methylionone reached 79.9%,and content was above 91.8%,the b.p.was 90～100℃/267～400Pa,n 20 D was 1.5000～1.5020. Renewable catalyst was used for 7 times and average yield of cyclization was 80.6%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
1998年第3期19-21,共3页
Fine Chemicals
