New technique for preparing alpha halogenate acid in class of optical purity
A preparation process and technology of halogenated acid, which is applied in the field of optically pure α-halogenated acid, can solve the problems of low optical purity, expensive resolution agent, and no practical application value, and achieve the effect of easy-to-obtain raw materials and simple process
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Embodiment 1
[0027] Put 45.12 grams of D-DBTA·H 2 O, 30.0 g of α-bromo-o-chlorophenylacetic acid dissolved in 300 ml of acetonitrile, add 48 g of copper acetate, stir at room temperature until the complex precipitates, add 150 ml of acetonitrile, continue to stir for 5 days, filter, the filter cake is washed with a small amount of acetonitrile , Dry, get 117 grams of complex. The complex was crushed, hydrolyzed with 1200 ml of 10% HCl, and filtered to obtain D-DBTA·H 2 O crude product, then in the D-DBTA·H 2 Add 100 ml of toluene to the crude product and stir vigorously for 15 minutes, filter to obtain 38 grams of pure product D-DBTA·H 2 O (recovery rate of 84.2%). The hydrochloric acid filtrate was extracted with 100 ml of ethyl acetate and extracted 3 times. The extract was combined with the above toluene layer, washed twice with saturated NaCl solution, dried with anhydrous sodium sulfate, filtered to remove sodium sulfate, and evaporated to dryness to obtain (+)-α -28.5 grams of crude brom...
Embodiment 2
[0031] To the recovered α-bromo-o-chlorophenylacetic acid in Example 1, 37.6 grams of recovered D-DBTA·H was added 2 O, the recovered 40 g of copper acetate and 375 ml of acetonitrile, dissolve and stir until the precipitated complex, then vigorously stir for 5 days, filter, wash the filter cake with a small amount of acetonitrile, and dry. The complex was crushed, dissociated with 800 ml of 10% HCl, and filtered to obtain D-DBTA·H 2 O crude product, then in the D-DBTA·H 2 Add 100 ml of toluene to the crude product and stir vigorously for 15 minutes and filter to obtain 28.59 g of pure product D-DBTA·H 2 O (recovery rate of 76.3%). The hydrochloric acid filtrate was extracted with 100 ml of ethyl acetate and extracted 3 times. The extract was combined with the above toluene layer, washed twice with saturated NaCl solution, dried with anhydrous sodium sulfate, filtered to remove sodium sulfate, and evaporated to dryness to obtain (+)-α -13.5 g of bromo-o-chlorophenylacetic acid wit...
Embodiment 3
[0035] To the recovered α-bromo-o-chlorophenylacetic acid in Example 2, 10 grams of recovered D-DBTA·H was added 2 O, 27.2 g of copper acetate and 300 ml of acetonitrile recovered, dissolved and stirred until the complex precipitated, stirred vigorously for 5 days, filtered, the filter cake was washed with a small amount of acetonitrile, and dried to obtain 31 g of the complex. , Filter with 350 ml 10% HCl to get D-DBTA·H 2 O crude product, then in the D-DBTA·H 2 Add 50 ml of toluene to the crude product and stir vigorously for 15 minutes, filter to obtain 13.5 g of pure product D-DBTA·H 2 O. The hydrochloric acid filtrate was extracted with 50 ml of ethyl acetate and extracted 3 times. The extract was combined with the above toluene layer, washed twice with saturated NaCl solution, dried with anhydrous sodium sulfate, filtered to remove sodium sulfate, and evaporated to dryness to obtain 2.5 g (+) -α-Bromo-o-chlorophenylacetic acid with an optical purity of 81.2%ee. The crude pro...
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