Application of a Combination Catalyst in Specific Friedel-Crafts Reaction
A combination catalyst and Friedel-Crafts reaction technology, which is applied in the direction of physical/chemical process catalysts, condensation preparation of carbonyl compounds, organic chemistry, etc., can solve the problems of high price, poor effect, poor selectivity of Friedel-Crafts reaction speed, etc., and achieve reduction The use of inorganic salts, the effect of improving quality and yield, and reducing process costs
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Embodiment 1
[0058] Example 1: Preparation of (5-bromo-2-chlorophenyl)(4-ethoxyphenyl)methanone
[0059]
[0060] Referring to the technology described in patent WO2009026537: 15g of 5-bromo-2-chlorobenzoic acid (0.064mol), 100mL of dichloromethane and 0.5mL of N,N-dimethylformamide were sequentially added to a 250mL three-necked flask, and the mixture was stirred and mixed. uniform. 8.1 g of oxalyl chloride (0.064 mol, 1.0 eq) was added dropwise to the uniformly stirred mixture at 20-30° C., and the resulting mixture was stirred at room temperature overnight. The reaction solution was transferred to a 250 mL round-bottomed flask, concentrated to dryness under reduced pressure at 35-45 °C, and 50 mL of dichloromethane was added to dissolve and concentrate the resulting slurry, and the clear solution was 5-bromo-2-chlorobenzoyl chloride solution, spare.
[0061] 7.8 g of phenethyl ether (0.064 mol, 1.0 eq) and 50 mL of dichloromethane were sequentially added to a 250 mL three-necked fl...
Embodiment 2
[0064] Example 2: Preparation of (5-bromo-2-chlorophenyl)(4-ethoxyphenyl)methanone
[0065]
[0066] Application of the technical solution of the present invention: 15g of 5-bromo-2-chlorobenzoic acid (0.064mol), 100mL of dichloromethane and 0.5mL of N,N-dimethylformamide were sequentially added to a 250mL three-necked flask, and the mixture was stirred and mixed. uniform. 8.1 g of oxalyl chloride (0.064 mol, 1.0 eq) was added dropwise to the uniformly stirred mixture at 20-30° C., and the resulting mixture was stirred at room temperature overnight. The reaction solution was transferred to a 250 mL round-bottom flask, concentrated to dryness under reduced pressure at 35-45° C., and 50 mL of dichloromethane was added to dissolve and concentrate the resulting slurry, and the clear solution was used for later use.
[0067]7.8 g of phenethyl ether (0.064 mol, 1.0 eq) and 50 mL of dichloromethane were sequentially added to a 250 mL three-necked flask, stirred and mixed, and the...
Embodiment 3
[0070] Example 3: Preparation of (5-bromo-2-chlorophenyl)(4-ethoxyphenyl)methanone
[0071]
[0072] Friedel-Crafts acylation reaction under the catalysis of ferric chloride: 15g of 5-bromo-2-chlorobenzoic acid (0.064mol), 100mL of dichloromethane and 0.5mL of N,N-dimethylmethane were successively added to a 250mL three-necked flask. amide, and stir to combine. 8.1 g of oxalyl chloride (0.064 mol, 1.0 eq) was added dropwise to the uniformly stirred mixture at 20-30° C., and the resulting mixture was stirred at room temperature overnight. The reaction solution was transferred to a 250 mL round-bottom flask, concentrated to dryness under reduced pressure at 35-45° C., and 50 mL of dichloromethane was added to dissolve and concentrate the resulting slurry, and the clear solution was used for later use.
[0073] 7.8 g of phenethyl ether (0.064 mol, 1.0 eq) and 50 mL of dichloromethane were sequentially added to a 250 mL three-necked flask, stirred and mixed, and the mixture wa...
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