Preparation method of esculene mesylate impurity
A technology for methanesulfonic acid and impurities, which is applied in the field of synthesis of pharmaceutical impurities, can solve problems such as affecting the quality of pharmaceuticals, and achieve the effects of simple post-processing and mild reaction conditions.
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Embodiment 1
[0021]
[0022] Add 1.0 g of compound I-A to the reaction flask, then add 20 g of dichloromethane, 0.5 g of 2,4,6-collidine, and 0.01 g of pyridine. Then, 0.21 g of benzoyl chloride was added dropwise at an internal temperature of 0°C. After reacting for 0.5 hour, 20 g of water and 20 g of dichloromethane were added, and the layers were separated. The organic layer was spin-dried to obtain I-B-1.
[0023]
[0024] Add 1.14g of compound I-B-1 to the reaction flask, then add 22.8g of dichloromethane, 0.86g of pyridine, and 0.95g of methanesulfonic anhydride, then magnetically stir at room temperature, react for 0.5 hours, add 30g of water, and separate layers. The aqueous phase was back-extracted with 21 g of dichloromethane, and the combined organic phases were concentrated under reduced pressure to obtain 1.25 g of compound I-C-1.
[0025]
[0026] Add 1.25g compound I-C-1 to the reaction flask, then add 63ml DMF, 0.27gNaN 3 , 0.01 g pyridine. Then control the int...
Embodiment 2
[0033]
[0034] Add 1.0 g of compound I-A to the reaction flask, then add 20 g of dichloromethane, 0.5 g of 2,4,6-collidine, and 0.01 g of pyridine. Then, 0.12 g of acetyl chloride was added dropwise at an internal temperature of 0°C. After reacting for 0.5 hour, 20 g of water and 20 g of dichloromethane were added, and the layers were separated. The organic layer was spin-dried to obtain I-B-2.
[0035]
[0036] Add 1.04g of compound I-B-2 to the reaction flask, then add 22.8g of dichloromethane, 0.86g of pyridine, and 0.95g of methanesulfonic anhydride, then magnetically stir at room temperature, and react for 0.5 hours. Add 30g of water and separate layers. The aqueous phase was back-extracted with 21 g of dichloromethane, and the combined organic phases were concentrated under reduced pressure to obtain 1.13 g of compound I-C-2.
[0037]
[0038] Add 1.13g compound I-C-2 to the reaction flask, then add 63ml DMF, 0.27gNaN 3 , 0.01 g pyridine. Then control the i...
Embodiment 3
[0044]
[0045]Add 1.0 g of compound I-A to the reaction flask, then add 20 g of dichloromethane, 0.5 g of 2,4,6-collidine, and 0.01 g of pyridine. Then, 0.21 g of benzoyl chloride was added dropwise at an internal temperature of 0°C. After reacting for 0.5 hour, 20 g of water and 20 g of dichloromethane were added, and the layers were separated. The organic layer was spin-dried to obtain I-B-1.
[0046]
[0047] Add 1.13g of compound I-B-1 to the reaction flask, then add 22.8g of dichloromethane, 0.86g of pyridine, and 1.77g of p-toluenesulfonic anhydride, then magnetically stir at room temperature and react for 0.5 hours. Add 30g of water and separate layers. The aqueous phase was back-extracted with 21 g of dichloromethane, and the combined organic phases were concentrated under reduced pressure to obtain 1.35 g of compound I-C-3.
[0048]
[0049] Add 1.35g compound I-C-3 to the reaction flask, then add 63ml DMF, 0.27gNaN 3 , 0.01 g pyridine. Then control the ...
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