药物中间体4-苄氧基-3-氯苯胺的合成

Synthesis of drug intermediate 4-benzyloxy-3-chlorobenzenamine

选用无水碳酸钾做缚酸剂,DMF做溶剂,由4-硝基-2-氯苯酚和氯苄制备4-苄氧基-3-氯硝基苯,进而,4-苄氧基-3-氯硝基苯在催化剂六水合三氯化铁/活性炭,还原剂80%水合肼,溶剂乙醇的作用下得到目标产物,着重考察了反应时间,反应温度,物料物质的量配比对目标产物收率的影响,确定了合成最佳条件为反应温度80℃,反应时间3 h,n(4-苄氧基-2-氯硝基苯)∶n(水合肼)=8∶1,在此条件下,目标化合物收率83.6%,两步总收率收率77.8%,产物经过1HNMR和MS确认.

Firstly,4-benzyloxy-3-chloro-1-nitrobenzene was synthesized from benzyl chloride and 2-chloro-4-nitrophenol using potassium carbonate as an acid binding agent in DMF. Seondly,with Fe Cl3·6H2O-Pd/C as a catalyst and 80% NH2·NH2as an reducing agent in ethanol,4-benzyloxy-3-chlorobenzenamine was synthesized from 4-benzyloxy-3-chloro-1-nitrobenzene. The reaction temperature,reaction time and mole ratios on the yield of the target product were investigated. The optimum condition was given as follows: the reaction temperature of 80 ℃,reaction time of 3 h,the mole ratio of80% hydrazine to 4-benzyloxy-3-chloronitrophenoxyl = 8 ∶ 1,and the yield of target compound was83.6%. the total yield was about 77.8% with two steps. The target compound was determined by1 HNMR and MS.