Method for producing 1,3-bisacyloxy-2-methylene propane
一种亚甲基丙烷、制造方法的技术，应用在1领域，能够解决没有记载制造等问题，达到生产效率和成本改善的效果
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preparation example Construction
[0083] As the catalyst obtained by the above-mentioned production method, it is preferable that the specific surface area is 10 to 250 m 2 / g, a catalyst with a pore volume of 0.1-1.5mL / g.
[0084] The ratio of palladium in the catalyst to the carrier is preferably 10 to 1000 parts by mass of the carrier, more preferably 30 to 500 parts by mass, relative to 1 part by mass of palladium. When the carrier is 10 parts by mass or more with respect to 1 part by mass of palladium, the dispersion state of palladium improves and the reaction performance improves. Moreover, industrial applicability improves by making a carrier into 1000 mass parts or less with respect to 1 mass part of palladium.
[0085] The amount of the catalyst used in the production method of the present invention is not particularly limited, but from the viewpoint of improving production efficiency, it is preferably 0.01 to 20% by mass, more preferably 0.1 to 20% by mass, based on the total mass of carboxylic aci...
Embodiment
[0111] Hereinafter, although an Example and a comparative example demonstrate this invention more concretely, this invention is not limited to these Examples and a comparative example.
[0112] 〔Analysis conditions〕
[0113] The solution (reaction mixture) after the reaction was analyzed using a gas chromatograph GC2014 (FID detector manufactured by Shimadzu Corporation) and a capillary column (DB-1 manufactured by Agilent Technologies, length 30 m, inner diameter 0.25 mm, film thickness 0.25 μm) , under the following conditions.
[0114] Column temperature: 50°C (5 minutes) → 10°C / min → 250°C (5 minutes)
[0115] FID temperature: 250°C
[0116] Injection port temperature: 250°C
[0117] Carrier Gas: Helium
[0118] Supplementary Gas: Helium
[0119] Injection volume: 0.2μL
[0120] Column gas flow rate: 0.38mL / min
[0121] Split ratio: 20
manufacture example 1
[0122] [Manufacturing Example 1: Preparation of Catalyst 1]
[0123] Immerse 250mL (144g) of a silica carrier (5mmφ) in an aqueous solution containing 4.00g (13.6mmol) of sodium tetrachloropalladate and 3.90g (9.5mmol) of tetrachloroauric acid tetrahydrate to make it fully absorb water (Japanese : full water absorption). Next, 200 mL of an aqueous solution containing 16 g (131 mmol) of sodium metasilicate was added, and it was left still for 20 hours. Thereafter, 9.50 g (190 mmol) of hydrazine monohydrate was added to reduce the palladium salt and the gold salt to metal. After the reduced catalyst was washed with water, it was dried at 110° C. for 4 hours. Thereafter, the carrier containing the metal palladium was charged into an aqueous solution containing 13.34 g (136 mmol) of potassium acetate to absorb all the liquid, and then dried at 110° C. for 4 hours to prepare Catalyst 1 .
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