1,1,1,5,5,5-六氟乙酰丙酮 二水合物

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To the obtained crude 1,1,1,5,5,5-hexafluoroacetylacetone dihydrate 70 ml of toluene were added, followed by stirring for 1 hr at room temperature with a magnetic mixer, then filtration and then drying, thereby obtaining 27.3 g of 1,1,1,,5,5,5-hexafluoroacetylacetone dihydrate (see Table). A 100-ml glass reaction vessel, equipped with a thermometer, a stirrer and a reflux condenser filled with glass spheres, was charged with 27.3 g of the obtained 1,1,1,5,5,5-hexafluoroacetylacetone dihydrate and 55 g of 98% sulfuric acid, while nitrogen gas was allowed to flow through the reaction vessel. Then, the mixture was gradually heated to 80° C. with stirring by a magnetic mixer. During this heating, 21.0 g of a distillate of about 70° C. was collected. This distillate was found by the same gas chromatography as that of Example 1 to be 1,1,1,5,5,5-hexafluoroacetylacetone having a purity of 99.9%. were added filtration drying obtaining 27.3 g of 1,1,1,,5,5,5-hexafluoroacetylacetone dihydrate (see Table) equipped with a thermometer, a stirrer and a reflux condenser filled with glass spheres Then, the mixture was gradually heated to 80° C. with stirring by a magnetic mixer During this heating, 21.0 g of a distillate of about 70° C. was collected

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To the obtained crude 1,1,1,5,5,5-hexafluoroacetylacetone dihydrate 70 ml of toluene were added, followed by stirring for 1 hr at room temperature with a magnetic mixer, then filtration and then drying, thereby obtaining 27.3 g of 1,1,1,,5,5,5-hexafluoroacetylacetone dihydrate (see Table). A 100-ml glass reaction vessel, equipped with a thermometer, a stirrer and a reflux condenser filled with glass spheres, was charged with 27.3 g of the obtained 1,1,1,5,5,5-hexafluoroacetylacetone dihydrate and 55 g of 98% sulfuric acid, while nitrogen gas was allowed to flow through the reaction vessel. Then, the mixture was gradually heated to 80° C. with stirring by a magnetic mixer. During this heating, 21.0 g of a distillate of about 70° C. was collected. This distillate was found by the same gas chromatography as that of Example 1 to be 1,1,1,5,5,5-hexafluoroacetylacetone having a purity of 99.9%. were added filtration drying obtaining 27.3 g of 1,1,1,,5,5,5-hexafluoroacetylacetone dihydrate (see Table) equipped with a thermometer, a stirrer and a reflux condenser filled with glass spheres Then, the mixture was gradually heated to 80° C. with stirring by a magnetic mixer During this heating, 21.0 g of a distillate of about 70° C. was collected

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 100-ml glass reaction vessel, equipped with a thermometer, a stirrer and a reflux condenser filled with glass spheres, was charged with 12.5 g of the obtained 1,1,1,5,5,5-hexafluoroacetylacetone dihydrate and 25 g of 98% sulfuric acid, while nitrogen gas was allowed to flow through the reaction vessel. Then, the mixture was gradually heated to 80° C. with stirring by a magnetic mixer. During this heating, 9.5 g of a distillate of about 70° C. were collected. This distillate was found by the same gas chromatography as that of Example 1 to be 1,1,1,5,5,5-hexafluoroacetylacetone having a purity of 99.9%. equipped with a thermometer, a stirrer and a reflux condenser filled with glass spheres During this heating, 9.5 g of a distillate of about 70° C. were collected

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 20-ml eggplant-type flask was charged with 12.8 g of the obtained 1,1,1,5,5,5-hexafluoroacetylacetone dihydrate and 26.0 g of 98% sulfuric acid. Then, the flask was stopped, and the mixture was stirred for 4 hr at room temperature with a magnetic mixer, followed by standing still for 1 hr to have two layers separated from each other. Then, 9.8 g of 1,1,1,5,5,5-hexafluoroacetylacetone were obtained from the organic layer. This product was found by the same gas chromatography as that of Example 1 to be 1,1,1,5,5,5-hexafluoroacetylacetone having a purity of 99.9%. by standing still for 1 hr separated from each other

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 100-ml glass reaction vessel, equipped with a thermometer, a stirrer and a reflux condenser filled with glass spheres, was charged with 16.5 g of the obtained 1,1,1,5,5,5-hexafluoroacetylacetone dihydrate and 33.0 g of 98% sulfuric acid, while nitrogen gas was allowed to flow through the reaction vessel. Then, the mixture was gradually heated to 80° C. with stirring by a magnetic mixer. During this heating, 12.3 g of a distillate of about 70° C. were collected. This distillate was found by the same gas chromatography as that of Example 1 to be 1,1,1,5,5,5-hexafluoroacetylacetone having a purity of 99.9%. equipped with a thermometer, a stirrer and a reflux condenser filled with glass spheres During this heating, 12.3 g of a distillate of about 70° C. were collected

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 100-ml eggplant-type flask was charged with 16.2 g of the obtained 1,1,1,5,5,5-hexafluoroacetylacetone dihydrate and 33.0 g of 98% sulfuric acid. Then, the flask was stopped, and the mixture was stirred for 4 hr at room temperature with a magnetic mixer, followed by standing still for 1 hr to have two layers separated from each other. Then, 12.5 g of 1,1,1,5,5,5-hexafluoroacetylacetone were obtained from the organic layer. This product was found by a gas chromatography (detector: FED, column: DB-1, column size: 0.25 mm×60 m) to be 1,1,1,5,5,5-hexafluoroacetylacetone having a purity of 99.9% (areal % in gas chromatography). by standing still for 1 hr separated from each other