Synthetic Route of 756520-66-8 , The common heterocyclic compound, 756520-66-8, name is 1-(2,6-Dichloro-3-fluorophenyl)ethanol, molecular formula is C8H7Cl2FO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
In a 100mL single-necked flask,1.2 g (0.005 mol) of 2-amino-4-hydroxy-6-bromo-quinazoline was added,(0.0065 mol, 1.3 equiv) of benzotriazol-1-yloxytris (dimethylamino) phosphonium hexafluorophosphate (BOP)Acetonitrile 20 mL,Stirred at room temperature,A solution of 1.1 mL (0.0075 mol, 1.5 equiv) of 1,8-diazabicycloundecyl-7- (DBU) was added to clarify the solution,After 10min reaction with solid precipitation,Join again1.56 g of 1- (3-fluoro-2,6-dichloro-phenyl) ethanol (0.0075 mol,1.5 equiv),0.4 g of NaH (60%) and 10 mL of acetonitrile,After stirring at room temperature overnight,Add 200mL H2O,Extract three times with 90 mL of ethyl acetate,Combine ethyl acetate,Evaporation of ethyl acetate,Got a white solid.The residue was purified by silica gel column chromatography (petroleum ether: dichloromethane: ethyl acetate = 2: 1: 2)Yield 55%.
The synthetic route of 756520-66-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Southern Medical University; Wan Shanhe; Wang Guangfa; Wu Xiaoyun; Tian Yuanxin; Ye Ling; Li Zhonghuang; Zhang Tingting; Zhu Zhengguang; Jin Hong; Zhang Jiajie; (27 pag.)CN106565684; (2017); A;,
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