摘要
对硝基苯甲酰氯和氯苯在无水三氯化铝催化下,生成4-硝基-4-氯二苯甲酮。通过多因素正交试验,确定最佳工艺条件为对硝基苯甲酰氯:氯苯:无水三氯化铝 = 1.0:2.0:1.3(mol),保温温度70℃,保温时间1.5h。收率为84.33%,含量99.36%。产品结构经红外光谱、核磁共振、质谱和元素分析测定证实。实验操作简单,分离容易。
nitro-4-chlorobenzphenone was prepared by the reaction of 4-nitrobenzoyl chloride with chlorobenzene under the catalysis of anhydrous alchlor. With the conditional tests, it is determined that the factors influencing the reaction is thermos temperature, thermos time, the amount of catalyst used and the ratio of 4-nitrobenzoyl chloride to chlorobenzene. The orthogonal experiment suggested that the optimal condition was 4-nitrobenzoyl chloride:chlorobenzene: anhydrous alchlor=1:2.0:1.3(mol), the thermos temperature 70℃, thermos time 1.5h. The effects of thermos temperature, thermos time, catalyst quantity and the ratio of 4-nitrobenzoyl chloride to chlorobenzene were discussed in detail. With the increase of the ratio of 4-nitrobenzoyl chloride to chlorobenzene the yield increases. Prolonging the thermos time is useful for the reaction, but the yield will not be increased evidently if the thermos time is longer than 1.5hours. From 50℃ to 70℃, the yield increases when the thermos temperature is inereased, and from 70℃ to 80℃, the yield decreases when the thermos temperature is increased. In the range of 1.3-1.4mol alchlor added, the yield decreases with the increasing of added alchlor, but in the range of 1.4-1.5mol alcohol added, the yield increases with increasing alchlor added. Of the four factors, the most influencing factor is the ratio of 4-nitrobenzoyl chloride to chlorobenzene; next is ithermos temperature and thermos time; and the least is catalyst quantity. The product is light yellow needle crystal, m.p101-103℃. The purity of product is 99.36%. and the yield is 84.33%. The structure of product was confirmed by IR, NMR, MS and EMA analyse. The purity of product was detected with HPLC. The operation of the experiment was very simple, and the product was separated easily.
出处
《高校化学工程学报》
EI
CAS
CSCD
北大核心
2002年第2期198-202,共5页
Journal of Chemical Engineering of Chinese Universities
基金
国家"九五"攻关项目。
