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A technology for prenol and butenol, applied in the field of synthesis of prenol, can solve problems such as inconvenience, and achieve the effects of cost reduction, broad prospects and low production cost
Active Publication Date: 2018-02-16
山东成泰新材料有限公司
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[0005]
In summary, there are obviously inconveniences and defects in the actual use of the existing technology, so it is necessary to improve
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Embodiment 1
[0017] Under a nitrogen atmosphere of 0.5MPa, add 650.0 grams of 3-methyl-3-buten-1-ol to the reactor, add 0.65 grams of aluminum isopropoxide, 0.65 grams of Na-Na 2 CO 3 / γ-Al 2 o 3 Solid super strong base, controlled temperature is 110°C, reaction time is 3h, filtered, detected by chromatograph, 468.0 g of 3-methyl-3-buten-1-ol participated in the reaction, and the final product isopentenol 442.6 grams, conversion rate 72.0%, selectivity 94.5%, yield 68.1%.
Embodiment 2
[0019] Under a nitrogen atmosphere of 1MPa, add 650.0 grams of 3-methyl-3-buten-1-ol to the reactor, add 0.43 grams of aluminum isopropoxide, 0.87 grams of Na-Na 2 CO 3 / γ-Al 2 o 3 Solid super base, controlled temperature is 120°C, reaction time is 2h, pumped and filtered, detected by chromatograph, 483.5 grams of 3-methyl-3-buten-1-ol participated in the reaction, and the final product isopentenol 439.9g gram, conversion rate 74.4%, selectivity 91.0%, yield 67.7%.
Embodiment 3
[0021] Under a nitrogen atmosphere of 4MPa, add 650.0 grams of 3-methyl-3-buten-1-ol to the reactor, add 13.5 grams of aluminum isopropoxide, 26.5 grams of Na-Na 2 CO 3 / γ-Al 2 o 3 Solid super strong base, controlled temperature is 120°C, reaction time is 2.1h, pumped and filtered, detected by chromatograph, 475.5 grams of 3-methyl-3-buten-1-ol participated in the reaction, and the final product isopentenol was generated 445.3 grams, selectivity 93.6%, conversion 73.2%, yield 68.5%.
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Abstract
The invention is suitable for the technical field of a synthetic method for isopentenol and provides a method for synthesizing isopentenol from butenol. The method is a method for isomerizing double bonds of 3-methyl-3-butenol under the catalytic action of a catalyst composed of solid super base and aluminium isopropoxide, wherein the solid super base is Na-Na2CO3 / gamma-Al2O3, the dosage of the catalyst is 0.2-12% of 3-methyl-3-butenol, and the mass ratio of the solid super base and aluminium isopropoxide in the catalyst is 1: 1 to 1: 2. The reaction pressure is 0.5-4MPa, the temperature is 100-140 DEG C and the time is 2-3 hours. The method provided by the invention is mild in reaction condition, the catalyst is high in activity and easy to separate and can be repeatedly used, the method is low in production cost, environmental-friendly and safe in production, and the product is high in purity and selectivity and green and environmental-friendly, so that the cost is greatly lowered, and the method is an efficient and economical synthetic method and has a wide prospect.
Description
technical field [0001] The invention relates to the technical field of synthesis methods of prenol, in particular to a method for synthesizing prenol from butenol. Background technique [0002] Superbase reagent is a kind of metallization reaction reagent mixed with organometallic compound and activator, which is widely used in the fields of basic organic synthesis, drug synthesis, electronic material research and development, etc. Compared with a single metallation reagent, it has many superior properties, its preparation method is simple, not only has a high base strength, but also makes the metallation reaction highly regioselective and stereochemically selective. As an environmentally friendly catalyst, solid base catalysts are widely used in organic synthesis and play an important role in process reform. Solid base catalysts form carbanions through electron accepting and accepting ligands to make the reaction happen. So far, great progress has been made in the research...
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