正交试验法优选盐酸对氯苯肼的合成工艺

OPTIMIZATION OF SYNTHETIC TECHNOLOGY OF p-CHLOROPHENYL- HYDRAZINE HYDROCHLORIDE BY ORTHOGONAL TEST

目的 优选一种盐酸对氯苯肼合成工艺。方法 采用正交设计 ,以对氯苯肼合成工艺中滴加盐酸时的温度 (A) ,滴加盐酸所用时间 (B)还原反应温度 (C)和还原反应的时间 (D)为 4个因素 ,每因素选取 3个水平进行试验 ,测定样品中杂质苯肼的含量。结果 因素A和C对杂质苯肼的含量均有显著影响 ,因素B和D影响不显著。优化合成工艺为A2 B1 C3D1 。

OBJECTIVE To seek the optimal synthetic technology of p-chlorophenylhydrazine hydrochloride by orthogonal test.METHODS According to the L 9(3 4)orthogonal table,four factors were selected.The temperature and the extended time of hydrocholoride dropping were factor A and B, respectively. The temperature and the expended time of reductive reaction were the factor C and D,respectively.Three levels of each factor were chosen and the contents of phenylhydrazine were assessed.RESULTS The factor A and C had significant effect on the content of phenylhydrazine,and the optimeal synthetic technology was A 2B 1C 3D 1.CONCLUSION It was feasible to select the optimal synthetic technology of p-chlorophenylhydrazine hydrochloride by orthogonal test.