Preparation method of 1-(4-chlorphenyl)-2-cyclopropyl-1-acetone
A cyclopropyl methyl ketone and cyclopropyl technology, which can be used in the preparation of carbon-based compounds, the preparation of organic compounds, and the compounds of elements in Group 4/14 of the periodic table, etc. Cyclopropaneacetic acid is expensive, difficult to separate and purify, etc., and achieves the effects of low reagent and medicine cost, low cost, and short time.
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Embodiment 1
[0027] (1) Dissolve 35.05g (0.1mol) α-trimethylsilyloxy diethyl p-chlorobenzyl phosphonate in 120mL N, N dimethylformamide, add 8.0g (0.2mol) sodium hydroxide , stirred and mixed evenly, slowly added dropwise 8.4g (0.1mol) cyclopropyl methyl ketone, controlled the temperature of the reaction system at 25°C, and continued to stir for 6 hours. The reaction solution was extracted with toluene, dried and precipitated to obtain 26.46g of Yellow oily liquid, namely 1-chloro-4-(2-cyclopropyl-1-trimethylsiloxypropen-1-yl)benzene, with a purity of 93.8% and a yield of 88.5%.
[0028] (2) 23.92g (0.08mol) of the finished product obtained in step (1), 50mL of toluene and 50mL of 15% hydrochloric acid were stirred at room temperature for 5 hours, extracted with toluene, and the organic layer was washed with water, dried, desolvated, and rectified Finally, 15.78 g of light yellow oily liquid, namely 1-(4-chlorophenyl)-2-cyclopropyl-1-propanone, was obtained with a purity of 97.8% and a yie...
Embodiment 2
[0031] (1) Dissolve 29.25g (0.1mol) of α-acetoxy dimethyl p-chlorobenzylphosphonate in 120mL of N-methylpyrrolidone, add 10.8g (0.2mol) of sodium methoxide, stir and mix evenly, and slowly drop 16.8g (0.2mol) of cyclopropyl methyl ketone, control the temperature of the reaction system at 20°C, stir continuously for 5 hours, extract the reaction solution with toluene, obtain 24.16g of light yellow oily liquid after drying and precipitation, that is, 1-chloro -4-(2-cyclopropyl-1-acetoxypropen-1-yl)benzene, purity 92.6%, yield 89.3%.
[0032] (2) 21.64g (0.08mol) of the finished product obtained in step (1), 50mL of toluene and 100mL of 15% p-toluenesulfonic acid solution were stirred at room temperature for 8 hours, extracted with toluene, and the organic layer was washed with water, dried and stripped. After dissolving and rectifying, 15.80 g of light yellow oily liquid, namely 1-(4-chlorophenyl)-2-cyclopropyl-1-propanone, was obtained with a purity of 98.2% and a yield of 93.0...
Embodiment 3
[0034] (1) Dissolve 32.85g (0.1mol) dimethyl α-methylsulfonyl p-chlorobenzylphosphonate in 120mL toluene solution, add 11.2g (0.2mol) potassium hydroxide, stir and mix evenly, slowly drop 12.6g (0.15mol) of cyclopropyl methyl ketone, control the temperature of the reaction system at 20°C, and continuously stir for 6 hours. The reaction solution is extracted with toluene, dried and precipitated to obtain 27.85g of light yellow oily liquid, namely 1-chloro -4-(2-Cyclopropyl-1-methylsulfonylpropen-1-yl)benzene, purity 93.1%, yield 90.5%.
[0035] (2) 24.62g (0.08mol) of the finished product obtained in step (1), 50mL of toluene and 50mL of 15% phosphoric acid were stirred at room temperature for 7 hours, extracted with toluene, and the organic layer was washed with water, dried, desolvated, and rectified Finally, 15.89 g of light yellow oily liquid, namely 1-(4-chlorophenyl)-2-cyclopropyl-1-propanone, was obtained with a purity of 96.9% and a yield of 92.3%.
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