Pharmaceutical Intermediates 2 - Amino - 6 - Bromo - Methoxy Phenol

2-nitro-4-methoxy-aniline,sodium hydroxide were used as the raw materials,after the three-step reaction,respectively for the Synthesis of 2-nitro-4-methoxyphenol,2-nitro-4-m ethoxy-6-brominephenol,2-amino-6-bromine-4-methoxyphenol.For the first synthesis of 2-nitro-4-methoxyphenol,2-nitro-4-methoxy-anili-ne,sodiu m hydroxide were used as the raw materials,then by bromine substitution reaction,we got 2-nitro-6-bromine-4-methoxyphenol.At last,by the reducing reaction,we got 2-amino-6-br omine-4-methoxyphenol.With the aid of the Infrared Absorption Spectroscopy(IR),Nude ar Magnetic Resonance Spectroscopy(NMR),Melting Point(M.P.),High Performance Liqu id Chromatogram(HPLC),etc,the structure of chemical compound synthesized were confi rmed and the purity was determined.Through designing the single factor experiment and o rthogonal experiment,the effects,such as reaction time,reaction temperature,solvent,etc, were discussed and better experiment conditions of every step were confirmed.The results showed that conversion ratio was up to 85.5%.For the first synthesis of 2-nitro-4-methoxyphenol,through single factor test and expe riment orthogonal,we have the best experimental conditions:the reaction temperature is 1 30℃,reaction time is 5h,10.0g4-methoxy-2-nitroaniline,6.0g sodium hydroxide,the volu me of water is 130mL.For the second synthesis of 2-nitro-6-bromine-4-methoxyphenol,through single factor test and experiment orthogonal,we have the best experimental conditions:reaction temper ature of 25℃,the reaction time 1.5h,2-nitro-4-methoxyphenol 5.6g,sodium acetate 5.5g,t he volume of bromine is 2.0mL.Confirmatory test,the results showed that conversion ratio was up to 71.3%,the purity of the pruduct was up to 88.4,after purification,the purity of t he pruduct was up to 98.8%.For the third of synthesis of 2-amino-6-bromine-4-methoxyphenol,through experime nts determine the feasibility of a better synthetic route:the reaction temperature is 80℃-85℃,the reaction time is 4h,the amount of Pd/C is 0.4g,the volume of hydrazine hydrate is 0.05mol,the results showed that conversion ratio was up to 85.5℃.