摘要
该反应以硫和硒作为催化剂,CO作为还原剂,在高温高压下还原1-硝基蒽醌制备1-氨基蒽醌。通过探究实验条件,选出了在底物量为6.00 g(27mmol)的前提下,确定了较优的反应条件:S 0.100 0 g(3.1 mmol);Se 0.015 8 g(0.2 mmol);Na HCO_3 2.00g;H_2O 40m L;反应温度150℃;压强PCO6 MPa;反应时间6h。高效液相色谱测得产物纯度最高可达98.18%。
1-Aminoanthraqinone was prepared from 1-nitroanthraqinone by high pressure reduction of CO/H2O in cyclohexane solvent in the presence of catalyst sulfur/selenium. The optimum condition was obtained by experiments： 1- nitroanthraquinone 6. 00 g（ 27mmol）,S 0.1500 g（ 0. 47 mmol）,Se 0. 0158 g（ 0. 20 mmol）,H2O 40 m L,Na HCO32. 00 g,temperature 150 ℃,PCO6.0 MPa and reaction time 6 hours. 1-Aminoanthraqinone yield was 98. 18%. The effect order of different factors for the reduction was gotten by orthogonal experiments L16（ 45） ： the amount of selenium powder 〉 reaction temperature〉CO gas pressure〉the amount of sulfur powder〉reaction time.
出处
《染料与染色》
CAS
2016年第6期28-30,42,共4页
Dyestuffs and Coloration
基金
辽宁省教育厅自然基金(12012002)
创新团队项目(LT2012001)
沈阳市重点实验室项目(F13-289-1-00)的资金支持
关键词
硫
一氧化碳
水相还原
1-氨基蒽醌
sulfur
monoxide carbon
aqueous reduction
1-aminoanthraqinone
