A kind of synthetic method of compound tulobuterol
A technology of tulobuterol and synthetic method, which is applied in the field of drug synthesis, can solve the problems of hidden safety hazards and high cost, and achieve the effects of improving production efficiency, less side reactions, and convenient use
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Embodiment 1
[0045] The preparation of embodiment 1 2-chlorostyrene
[0046] 78.3g (0.5mol) of 1-(2-chlorophenyl)-1-ethanol, 40.8g potassium bisulfate (0.3mol) and 5.5g hydroquinone (0.05mol) were added in a 500ml single-necked bottle, and then React at 190-195°C for 3 hours. After cooling down to room temperature, slowly pour the reaction system into 300ml of diethyl ether under stirring, spin the diethyl ether to dryness, add 200ml of dichloromethane and 100ml of water, stir well, separate the water layer, and wash the organic layer 3 times with saturated brine (50ml × 3), after drying, filtering and concentrating over anhydrous sodium sulfate, 61.2 g of 2-chlorostyrene was obtained as a colorless oil, with a yield of 88%.
Embodiment 2
[0047] The preparation of embodiment 2 2-chlorostyrene
[0048] 78.3g (0.5mol) of 1-(2-chlorophenyl)-1-ethanol, 54.5g potassium bisulfate (0.4mol) and 11.0g hydroquinone (0.1mol) were added in a 500ml single-necked bottle, and then React at 200-205°C for 3 hours. The aftertreatment method was the same as in Example 1 to obtain 62.6 g of the product, with a yield of 90%.
Embodiment 3
[0049] The preparation of embodiment 3 2-chlorostyrene
[0050] 78.3g (0.5mol) of 1-(2-chlorophenyl)-1-ethanol, 47.7g potassium bisulfate (0.35mol) and 8.3g hydroquinone (0.075mol) were added in a 500ml single-necked bottle, and then React at 210-215°C for 3 hours. The post-treatment method was the same as in Example 1 to obtain 58.4 g of the product, with a yield of 84%.
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