Method for preparing 1,1,1-trifluoroacetone
A technology of trifluoroacetone and ethyl trifluoroacetoacetate, which is applied in the field of preparation of 1,1,1-trifluoroacetone, can solve problems such as difficulty in industrialization and expensive catalysts, and achieve reduction of three wastes emissions, safe and reliable production process, Simple operation effect
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Embodiment 1
[0030] Add methanesulfonic acid (100.9g, 1.05mol) into a 150mL cold trap equipped with an electric stirring device, a thermometer, a constant pressure dropping funnel and a reflux condenser (the reflux condenser is connected to tap water, and the upper outlet is connected to a 150mL cold trap at -40°C) in a 250mL four-neck flask to collect the product). The methanesulfonic acid was heated to 100°C within 30 minutes, and ethyl 4,4,4-trifluoroacetoacetate (92.1 g, 0.5 mol) in a constant pressure dropping funnel was added dropwise to the methanesulfonic acid, During the dropwise addition, 1,1,1-trifluoroacetone was generated and collected in a cold trap at -40°C. After dripping, keep at 100°C for 1 hour, then rise to 110°C for 2 hours and then stop the reaction. 52.2g of colorless liquid is obtained as the product 1,1,1-trifluoroacetone with a purity of 99.1% (GC area Normalization method), the reaction yield was 92.4%.
[0031]
Embodiment 2
[0033] Add methanesulfonic acid (505g, 5.25mol) into a 500mL container equipped with an electric stirring device, a thermometer, a constant pressure dropping funnel and a reflux condenser (the reflux condenser is connected to tap water, and the upper outlet is connected to -40°C with a tube). Secondary cold trap to collect the product) in a 1 L four-necked flask. The methanesulfonic acid was heated to 100°C within 60 minutes, and ethyl 4,4,4-trifluoroacetoacetate (460.5 g, 2.5 mol) in the constant pressure dropping funnel was added dropwise into the methanesulfonic acid, During the dropwise addition, 1,1,1-trifluoroacetone was generated, which was collected in a secondary cold trap at -40°C. After dripping, keep at 100°C for 2 hours, and then rise to 110°C for 3 hours to stop the reaction. Receive 199.5g in the first-stage cold trap and 63.8g in the second-stage cold trap, a total of 263.3g of colorless liquid is The product 1,1,1-trifluoroacetone has a purity of 99.0% (G...
Embodiment 3
[0036] Add methanesulfonic acid (96g, 1.0mol) into a 150mL cold trap equipped with an electric stirring device, a thermometer, a constant pressure dropping funnel and a reflux condenser (the reflux condenser is connected to tap water, and the upper outlet is connected to a 150mL cold trap at -40°C) to collect the product) in a 250mL four-necked flask. The methanesulfonic acid was heated to 100°C within 30 minutes, and ethyl 4,4,4-trifluoroacetoacetate (100 g, 0.54 mol) in the constant pressure dropping funnel was added dropwise to the methanesulfonic acid, and During the addition process, 1,1,1-trifluoroacetone was generated and collected in a cold trap at -40°C. After dripping, keep at 100°C for 1 hour, and then rise to 110°C for 2 hours to stop the reaction. 49.7g of colorless liquid is obtained as the product 1,1,1-trifluoroacetone with a purity of 99.4% (GC area Normalization method), the reaction yield was 88.2%.
[0037]
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