尿素工艺法合成结晶紫内酯的研究

将一定比例的尿素、对二甲氨基苯甲醛、N,N-二甲基苯胺溶解在盐酸溶液中,在氮气保护下,于80℃左右反应0.5 h,再加入间二甲氨基苯甲酸于93℃左右搅拌回流5.5 h,得无色结晶紫内酯(LCVL),收率为65.00%。把LCVL溶解在碱性溶液中,以铁氰化钾为催化剂,通入空气反应18 h,得结晶紫内酯(CVL),收率为90.50%。讨论了萃取剂、温度、NaOH的质量与浓度及反应时间对反应的影响。

Synthesis of crystal violet lactone with urea technology

LCVL was prepared by heating a certain ratio of urea,p-dimethylaminobenzaldehyde and N,N-dimethylaniline mixed and refluxed in the hydrochloric acid and under the protection of nitrogen at about 80 ℃ for 0.5 h,then react 5.5 h in the presence of m-dimethylaminobenzoic acid at about 93 ℃ with 65% yield of LCVL.With potassium ferricyanide used as catalyst,LCVL dissolved in sodium hydroxide was oxidized to CVL by inpouring the air for 18 h.The yield of CVL is 90.50%.The effect of the extractant,temperature,weight and consistency of sodium hydroxide as well as time on the reaction were discussed.