77-68-9Relevant articles and documents
Synthesis of alcohol ester 12 in 1, 8-diazabicyclo [5.4.0] undec-7-ene (DBU)-based Self-separation catalytic system
Lv, Zhiguo,Zhang, Shuying,Guo, Zhenmei,Cheng, Xi,Wang, Jiaomei,Zhang, Chao
, (2019)
The synthesis of alcohol ester 12 is one of the valuable industrial processes, but it was impeded by poor separating property and recycling ability of the catalytic systems. Herein, four novel DBU-based basic ionic liquids (DBILs) of [BDBU]IM, [BDBU]OH, [ODBU]IM, [[ODBU]OH were synthesized successfully by introducing the alkyl chains of 1-bromobutane or 1-bromooctane to 1,8-diazabicyclo [5.4.0] undec-7-ene (DBU), and then, employing imidazole (IM?) or hydroxide (OH?) as counter ions. The above obtained four ionic liquids were applied in the synthesis of alcohol ester 12 in isobutyraldehyde (IBD)/aqueous media for the first time. Interestingly, after reaction, production of alcohol ester 12 can be self-separated from ionic liquids/water (ILs/W) catalytic system automatically. Furthermore, the self-separated ILs/W can be recycled and used in next catalytic reaction for at least 5 times without obvious loss of catalytic performance. In this work, the structure, purity, thermal stability and alkalinity of DBILs were characterized systematically. [BDBU]IM shows high alkalinity and thus enhances yield of 66.17%. From thermo gravimetric analyzer (TGA), [BDBU]IM also exhibits excellent thermal stability. So [BDBU]IM was chosen for the further studying. Furthermore, quantum chemistry is applied to calculate the interaction forces and electron energies of reactants by DFT, and the calculation results illustrate the feasibility of synthetic process of DBILs. The self-separation strategy of DBILS in this work may open up a new avenue for the clean synthesis of other industrial products.
Method for synthesis of 2, 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate
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Paragraph 0012-0018, (2018/03/26)
The invention discloses a method for one-step direct synthesis of 2, 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate from isobutyraldehyde in the presence of a strong basic ionic liquid as a catalyst.The method comprises that isobutyraldehyde undergoes aldol condensation and Cannizzaro reaction through one step in the presence of a strong basic ionic liquid as a catalyst to produce 2, 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate. The method solves the problems of toxicity and corrosion of an inorganic base catalyst and complicated processes of the two-stage reaction and realizes high product selectivity, few by-products, simple processes, energy saving, emission reduction and catalyst recycling.
Method for preparing 2, 2, 4-trimethyl-1, 3-pentanediol double isobutyric acid ester
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Paragraph 0028; 0029; 0030, (2016/11/28)
The invention discloses a method for preparing 2, 2, 4-trimethyl-1, 3-pentanediol double isobutyric acid ester. The method includes the steps that 1, an alkali metal hydroxide, a phase transfer catalyst and water are mixed in a certain proportion, and isobutyraldehyde is dropwise added slowly; the temperature is raised to 30-50 DEG C after the isobutyraldehyde is dropwise added completely, and heat preservation is conducted for 1-5 hours; 2, the temperature is lowered to room temperature, a water phase is removed, the alkali metal hydroxide is added to an organic phase in a certain proportion, the temperature is raised to 60-70 DEG C, and a heat preservation reaction is conducted for 6-12 hours; 3, the temperature is lowered to the room temperature, the alkali metal hydroxide is removed, and the remaining organic phase is reserved; 4, a certain quantity of isobutyric acid, a solid sulfate catalyst and a water-carrying agent are added to the remaining organic phase, the mixture is heated to 120-150 DEG C, and a heat preservation reaction is conducted for 2-5 hours; after the reaction is completed, filtering is conducted to remove the solid sulfate catalyst, water washing is conducted to remove isobutyric acid which does not participate in the reaction, the water-carrying agent is removed through rotary evaporation, reduced pressure distillation is conducted, and a target product is obtained. Compared with the prior art, by means of the preparation method, the target product is high in yield, the operation process is simple and safe, and industrialized production is achieved easily.