Preparation method of 5-bromo-2-chloro-4 '-ethoxydiphenylmethane
A technology of ethoxydiphenylmethane and ethoxybenzophenone, which is applied in the field of drug synthesis, can solve the problems of highly toxic cyanide and serious pollution, so as to improve reaction efficiency, reduce production costs, and reduce public project expenditures Effect
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preparation example Construction
[0022] A preparation method of 5-bromo-2-chloro-4'-ethoxydiphenylmethane is characterized in that it comprises the following steps:
[0023] Step S1, preparation of 5-bromo-2-chlorobenzoyl chloride: add 5-bromo-2-chlorobenzoic acid into dichloromethane, stir in an ice-water bath for 20-30 minutes, then add oxalyl chloride dropwise, The dropwise addition is completed within 1-2 hours. After the dropwise addition, the reaction is stirred at the first reaction temperature for 8-10 hours, and then the solvent and unreacted reactants are removed by rotary evaporation to obtain 5-bromo-2-chlorobenzoyl chloride; And the substance removed by rotary evaporation is recovered by condensation and reused as a solvent;
[0024] Step S2, the preparation of 5-bromo-2-chloro-4'-ethoxybenzophenone: 5-bromo-2-chlorobenzoyl chloride prepared through step S1, half weight of Friedel-Crafts acylation catalyst Add it into dichloromethane, stir and react in the ice-water mixture for 1-2 hours, then a...
Embodiment 1
[0035] Embodiment 1 provides a kind of preparation method of 5-bromo-2-chloro-4'-ethoxydiphenylmethane, it is characterized in that, comprises the following steps:
[0036] Step S1, Preparation of 5-bromo-2-chlorobenzoyl chloride: Add 5-bromo-2-chlorobenzoic acid into dichloromethane, stir in an ice-water bath for 20 minutes, then add oxalyl chloride dropwise for 1 hour After the dropwise addition, the reaction was stirred and reacted at the first reaction temperature for 8 hours after the dropwise addition, and the solvent and unreacted reactants were removed by rotary evaporation to obtain 5-bromo-2-chlorobenzoyl chloride; and the rotary evaporation was removed The substance is recovered by condensation and reused as a solvent;
[0037] Step S2, the preparation of 5-bromo-2-chloro-4'-ethoxybenzophenone: 5-bromo-2-chlorobenzoyl chloride prepared through step S1, half weight of Friedel-Crafts acylation catalyst Add it into dichloromethane, stir and react in the ice-water mixt...
Embodiment 2
[0045] Example 2 provides a method for preparing 5-bromo-2-chloro-4'-ethoxydiphenylmethane, which is basically the same as in Example 1, except that the 5-bromo-2- The molar ratio of chlorobenzoic acid, dichloromethane, and oxalyl chloride is 1:7:1.8; the first reaction temperature is 17°C; the 5-bromo-2-chlorobenzoyl chloride, Friedel-Crafts acylation described in step S2 The mol ratio of catalyzer, methylene chloride, phenetole is 1:1.3:5:1; Described Friedel-Crafts acylation catalyst is made of anhydrous aluminum chloride, anhydrous cupric chloride, anhydrous zinc chloride, lanthanum chloride Cerium is mixed at a mass ratio of 1:0.5:1:0.15.
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