Method for preparing 7-chloro-2,3,4,5-tetrahydro-1H-1-benzazepino-5-ketone
A technology for benzoazepines and zebralines is applied in the field of preparation of benzoazepines, can solve the problems of high cost, low yield, and cannot be well applied to industrialized production, and achieves the effect of reducing industrial costs
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Embodiment 1
[0037] p-Chloroaniline (89.3g, 0.70mol) and dichloromethane (250mL) were placed in a 2L reaction flask, and pyridine (60.9g, 62.3mL, 0.77mol) was added. The reaction solution was cooled to 0-5°C in an ice-water bath, and a solution of p-toluenesulfonyl chloride (139.2 g, 0.73 mol) and dichloromethane (250 mL) was added dropwise with stirring, and the drop was completed within 1 h. After dropping, the reaction was stirred at room temperature for 10 h. Water (500 mL) was added to the reaction solution, stirred for 10 min, and the layers were separated. The aqueous layer was extracted once with dichloromethane (100 mL). The organic layers were combined, washed with saturated brine (400 mL), and dried over anhydrous sodium sulfate. Dichloromethane was evaporated to dryness under reduced pressure, the resulting solid was added to methanol (400mL) and heated to dissolve, cooled to 0-5°C, slowly added water (400mL), kept stirring at 0-5°C for 30min, filtered, and cooled a little to...
Embodiment 2
[0039] p-Chloroaniline (89.3g, 0.70mol) and dichloromethane (250mL) were placed in a 2L reaction flask, and pyridine (55.4g, 56.6mL, 0.70mol) was added. The reaction solution was cooled to 0-5°C in an ice-water bath, and a solution of p-toluenesulfonyl chloride (160.2 g, 0.84 mol) and dichloromethane (250 mL) was added dropwise with stirring, and the drop was completed within 1 h. After dropping, the temperature was raised to dichloromethane reflux, and the reaction was stirred for 7h. Water (500 mL) was added to the reaction solution, stirred for 10 min, and the layers were separated. The aqueous layer was extracted once with dichloromethane (100 mL). The organic layers were combined, washed with saturated brine (400 mL), and dried over anhydrous sodium sulfate. Dichloromethane was evaporated to dryness under reduced pressure, the resulting solid was added to methanol (400mL) and heated to dissolve, cooled to 0-5°C, slowly added water (400mL), kept stirring at 0-5°C for 30m...
Embodiment 3
[0041] p-Chloroaniline (89.3g, 0.70mol) and dichloromethane (250mL) were placed in a 2L reaction flask, and pyridine (83.0g, 85.0mL, 1.05mol) was added. The reaction solution was cooled to 0-5°C in an ice-water bath, and a solution of p-toluenesulfonyl chloride (152.5 g, 0.80 mol) and dichloromethane (250 mL) was added dropwise with stirring, and the drop was completed within 1 h. After dropping, the temperature was raised to dichloromethane reflux, and the reaction was stirred for 5h. Water (500 mL) was added to the reaction solution, stirred for 10 min, and the layers were separated. The aqueous layer was extracted once with dichloromethane (100 mL). The organic layers were combined, washed with saturated brine (400 mL), and dried over anhydrous sodium sulfate. Dichloromethane was evaporated to dryness under reduced pressure, the resulting solid was added to methanol (400mL) and heated to dissolve, cooled to 0-5°C, slowly added water (400mL), kept stirring at 0-5°C for 30m...
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