| The materials4-Hydroxy-2,2-dimethyl-4-(2-thiazol)-cyclohexanecarboxylic acid and3-methyl-5-(4-trifluoromethyl-pyrimidin-2-ylamino)-bromobenzene were charged to get4-Hydroxy-2,2-dimethy1-4-{5-[3-methyl-5-(4-trifluoromethyl-pyrimidin-2-ylamino)-phenyl]-t hiazol-2-yl}-cyclohexanecarboxylic acid by Heck reation.By the reaction mechanism, Pd(II) connect SM1, then get the intermediate1, and SM2can get to intermediate2by base. At last, intermediate1and intermediate2can get the product A, then complex Pd(II) turn to Pd(II) for the next step.This paper is based on the different conditions to reduce production cost, and make the product yield maximize, then get the suitable industrial process.The product A is got by SM1and SM2, and the auxiliary raw materials are0.9X(1.66eq.) K2CO3,10.0X DMF,0.02X(0.3eq.) H2O,0.02X(0.02eq.) Pd(AcO)2and0.15X(0.1eq.) Butyldi-1-adamantylphosphine.Then SM1is1.0X(1.0eq.), SM2is1.2X(0.95eq.), X is based as SM1, and the temperature is110℃.After the reaction conditions confirmed, in order to ensure normal production under the condition, test certificate corresponding also to be carried out, finally succeeded in getting suitable process in factory. |
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