1,3-DICHLORO-5-(CHLOROMETHYL)BENZENE synthesis

Yield:3290-06-0 98.8%

Reaction Conditions:

Stage #1:3,5-dichlorobenzoic acid with sodium tetrahydroborate in tetrahydrofuran at 60; for 0.2 h;Inert atmosphere;
Stage #2: with potassium chloride in tetrahydrofuran at 110; under 1520.1 Torr; for 4 h;Sonication;Inert atmosphere;Temperature;Reagent/catalyst;Solvent;Pressure;

Steps:

1 Example 1
The method for synthesizing 3,5-dichlorobenzyl chloride includes the following steps:1) Under a argon atmosphere, add 1 mol of 3,5-dichlorobenzoic acid, anhydrous THF and sodium borohydride to the reaction vessel.The temperature was raised to 60 ° C for 12 min, potassium chloride, polyethylene glycol 200 and sodium hydroxide aqueous solution of pH=14 were added to start ultrasonic assist, and the ultrasonic power and frequency were 420 W and 60 KHz, respectively.The control temperature is 110 ° C, the reaction pressure is maintained at 2 atmospheres, and the reaction is completed for 4 hours;The ratio of 3,5-dichlorobenzoic acid to sodium borohydride and potassium chloride is 1:0.42:1.4; 3,5-dichlorobenzoic acid and anhydrous THF,The amount ratio of the aqueous sodium hydroxide solution was 1 mmol: 2 ml: 0.8 ml.2) After cooling the system, about 2 times the volume of the reaction solution of ethyl acetate is added, the insoluble matter is removed by filtration, and the layers are separated. The organic phase is dried over anhydrous magnesium sulfate and concentrated.Recrystallization gave the product in a molar yield of 98.8% and HPLC purity 98.1%.

References:

Shandong Nong Pharmaceutical Xue Institute;Jinan Kehai Co., Ltd.;Fu Hongxin;Yang Chaohui;Wang Ling CN109232164, 2019, A Location in patent:Paragraph 0008; 0026-0048

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