Synthetic method of bosutinib intermediate
A technology of bosutinib and a synthesis method, applied in the field of chemistry, can solve the problems of increased environmental protection pressure, difficult recycling and application, and high boiling point difference, and achieves the effects of convenient post-processing and purification, good reaction selectivity, and easy removal.
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[0037] Example 1
[0038] Synthesis method of bosutinib intermediate, bosutinib intermediate is 2,4-dichloro-5-methoxyaniline. In a 3000mL three-necked flask, add 545g of formic acid, turn on the stirring, and add m-aminophenol in batches 109g (1.0mol), 1.82g (10mmol) of vanadium pentoxide, heated to 100℃, TLC monitored the completion of the reaction (PE:EA=1:1), cooled to room temperature, in about 3h, chlorine gas was introduced to react, the color It turns to light yellow, and the reaction is completed monitored by dot plate (PE:EA=1:1). After the reaction is over, it is filtered, and the filtrate is recycled for recycling. The intermediate is directly subjected to the next reaction without purification. Add 1500mL of dimethylformamide and 207.3g (1.5mol) of potassium carbonate to the reaction flask containing 2,4-dichloro-5-carboxamidophenol from which formic acid has been recovered. Stir for 30min at 40℃, and add dropwise for about 1h. 189.2 g (1.5 mol) of dimethyl sulfat...
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[0041] Example 2
[0042] Into a 3000mL three-necked flask, add 1417g of formic acid, start stirring, add 109g (1.0mol) of m-aminophenol and 16.2g (70mmol) of tungsten trioxide in batches, heat to 50℃, TLC monitors the completion of the reaction (PE:EA=1: 1), then cool to 20° C., cool to room temperature, add 337.4 g (2.5 mol) of sulfonyl chloride dropwise, after the dropwise addition, the color gradually changes to light yellow, and the dot plate monitors the completion of the reaction (PE:EA=1:1). After the reaction is over, it is filtered, and the filtrate is recycled for recycling. Add appropriate amount of dichloroethane to the reaction flask from which the formic acid has been recovered, dissolve it, wash with water until it is neutral, and concentrate to obtain crude 2,4-dichloro-5-carboxamidophenol. Without purification, proceed directly to the next reaction. Transfer all the obtained crude 2,4-dichloro-5-carboxamidophenol to a 3000mL autoclave, add 1090g of acetonitrile...
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[0044] Example 3
[0045] Into a 3000mL three-necked flask, add 1090g of formic acid, start stirring, add 109g (1.0mol) of m-aminophenol and 9.1g (50mmol) of vanadium pentoxide in batches, heat to 70℃, TLC monitors the completion of the reaction (PE:EA=1 :1), then cool to 40°C, add 175.3g (3.0mol) of sodium chloride in batches, add 510.2g (4.5mol) of 30% hydrogen peroxide dropwise within 30min, and monitor the completion of the reaction by TLC (PE:EA=1:1) After the reaction is over, filter and recycle formic acid from the filtrate. The intermediate is directly subjected to the next reaction without purification. Add 1500 mL of propanol, 165.9 g (1.2 mol) of potassium carbonate, and stirring for 30 min at 40°C into the 3000 mL reaction flask containing 2,4-dichloro-5-carboxamidophenol after the recovery of formic acid. 151.4 g (1.2 mol) of methyl ester, heated to 50° C., and continued stirring for 1 h to obtain a white suspension. Pour the reaction solution into an ice-water mi...
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