Abstract: Novel synthesis and optimal reaction conditions for 4-amino-6-nitroresorcinol hydrochloride（ANR•HCl），a key intermidiate of poly（p-phenylene-2,6-benzobisoxazole）（PBO），were systematically studied. Effect of solvent dosage，activated carbon and FeSO4•7H2O，molar ratio of hydrazine hydrate and reaction time were optimizied with an L18（2×37）orthogonal test and a 2nd step optimization. ANR•HCl was obtained with 90.7% yield and 94.1% purity by selective reduction of 4,6- dinitroresorcinol（DNR）under the optimized conditions of 10.0g of DNR，1.5 g activated carbon，1.0g of FeSO4•7H2O，6.62 g of 85% hydrazine hydrate and reflux for 1 h in 150 mL ethanol. The refined ANR•HCl was identified by FT-IR，1H NMR，13C NMR and MS. The current process has the advantages of excellent product stability，high-selectivity，less organic pollution，easy operation and so on.

摘要： 系统地研究了PBO关键中间体4-氨基-6-硝基间苯二酚盐酸盐（ANR•HCl）的合成新工艺及其优化条件，在初步探索实验的基础上，选用混合正交表L18（2×37）及5个影响因子，进行4,6-二硝基间苯二酚（DNR）选择还原、成盐合成ANR•HCl的正交优化实验，并进行二次调优实验。结果表明：在95%高置信度时活性炭用量影响显著，在对其进行再次单独调优实验后，合成出收率90.73%、HPLC纯度94.05%的ANR•HCl产品，相应优化条件为：10.0 g DNR以150 mL乙醇为溶剂，在1.5 gC/1.0g FeSO4•7H2O催化下用6.62 g 85%水合肼回流还原反应1 h。精制后产品经FT-IR、1H NMR、13C NMR及MS等定性确认，具有产品的稳定性好、还原过程选择性高，污染低及操作方便等特点。