2987-16-8Relevant articles and documents
Selective hydrogenation of 3,3-dimethylbutanoyl chloride to 3,3-dimethylbutyraldehyde with silica supported Pd nanoparticle catalyst
Li, Sifang,Chen, Guoqin,Sun, Lan
, p. 813 - 816 (2011)
A novel method for selective hydrogenation of 3,3-dimethylbutanoyl chloride (DMBC) to 3,3-dimethylbutyraldehyde (DMBA) with silica supported Pd nanoparticle catalyst (Pd/SiO2) is developed. The catalysts were characterized by Fourier transform infrared spectroscopy, X-ray powder diffraction, N2 physisorption and transmission electron microscopy. The performance of the Pd/SiO2 catalyst was compared with Pd/C and Pd/BaSO4 catalysts with or without being pretreated by quinoline-sulfur. The Pd/SiO2 catalyst activated at 80 °C by bubbling hydrogen in cyclohexane for 1 h showed the highest yield of DMBA. For 3 wt.% Pd/SiO2, the yield of DMBA reached 84.6%, which exhibited much higher value than Pd/C and Pd/BaSO4 catalysts.
Zimmerman,A.H. et al.
, p. 7203 - 7209 (1977)
Production process 3 and 3 - dimethyl butyraldehyde
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Paragraph 0031; 0035-0036; 0039-0040; 0043, (2020/11/13)
The invention belongs to the technical field of chemical synthesis and particularly relates to a production technology of 3,3-dimethylbutyraldehyde. The production technology sequentially comprises the following steps: S1, taking tert-butyl alcohol and ethylene as raw materials, taking n-hexane as a reaction solvent, and catalyzing by using sulfuric acid to synthesize 3,3-dimethyl butyl sulfate; S2, under the action of the catalyst, controlling the temperature to be 30 to 50 DEG C and hydrolyzing to obtain 3,3-dimethylbutanol; S3, performing catalyzed oxidation on the 3,3-dimethylbutanol by using an inhibitor 701 and dimethylethyl nitrite to obtain the 3,3-dimethylbutyraldehyde. The production technology has the advantages of safety, reliability, low cost, good reproducibility and high purity of a final product.
Synthesis technology used for preparing 3, 3-dimethylbutyraldehyde through micro-channel reaction
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Paragraph 0039-0046, (2019/10/10)
The invention belongs to the technical field of organic synthesis, and more specifically relates to synthesis technology used for preparing 3, 3-dimethylbutyraldehyde through micro-channel reaction. According to the synthesis technology, reaction is carried out in two micro-channel reactors connected in series; in a first micro-channel reactor, chloro-tert-butane and vinyl acetate are taken a raw materials, aluminium trichloride-dichloromethane system is taken as a catalyst to perform synthesis reaction, a reaction product is introduced into a second micro-channel reactor for mixing with OR water for hydrolysis reaction, an obtained hydrolysis product is subjected to extraction separation so as to obtain a 3, 3-dimethylbutyraldehyde crude product, and rectification is adopted to prepare the pure 3, 3-dimethylbutyraldehyde. The synthesis technology is scientific and reasonable; reaction condition accurate control is realized; synthesis is simple and convenient; production cost is low; purity is 99.5% or higher; the synthesis process is friendly to the environment; and the purity is high.
Preparation method for key intermediate of neotame--3,3-dimethylbutyraldehyde
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Paragraph 0030-0031, (2018/12/02)
The invention provides a preparation method for key intermediate of neotame--3,3-dimethylbutyraldehyde, comprising the following steps: under nitrogen protection in a vessel, organic solvent and a solid acid catalyst are added, tert-butyl chloride and aryl acid vinyl esters are dropped; through a thermal insulation reaction, the catalyst is filtered, the organic layer is decompressed and distilled, and alkali or acid is added for heating, backflow and hydrolysis to produce a crude product to be rectified to produce the final 3,3-dimethylbutyraldehyde product. The preparation method for the keyintermediate of neotame--3,3-dimethylbutyraldehyde has the advantages of low material cost and simple operation, moderate reaction conditions and less side reactions and is safe, environmentally friendly and beneficial for industrial production.
