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Catalyst and application thereof
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A technology of catalyst and supported catalyst, which is applied in the field of medicine and chemical industry
Active Publication Date: 2015-06-03
HUBEI BIO PHARMA IND TECHCAL INST
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However, current NHC metal complexes still need to be improved
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preparation example Construction
[0053] 2.1 The first method (denoted as Preparation Method A), includes the following steps:
[0054] (1) In the presence of anhydrous calcium chloride, the compound represented by formula II and the glyoxal aqueous solution are subjected to condensation reaction. After the reaction is completed, the calcium chloride is filtered out, the solvent is concentrated, and the resulting product is used for later use
[0055] H 2 N-R
[0056] (II)
[0057] Among them, the meaning of R is the same as that described above 1 And R 2 Has the same meaning;
[0058] (2) Dissolve N,N-dimethyldimethylamine in dichloroethane, stir in an ice bath, slowly add acetyl chloride dropwise, add the product obtained in step (1) after the dropwise addition is complete, and remove In an ice bath, the reaction was stirred at room temperature for 30 minutes, and then the reaction solution was concentrated under reduced pressure to obtain a crude product. Optionally, the obtained crude product was refined by recryst...
Embodiment 1-42
[0152] According to the details shown in Table 1, according to the preparation method described in the General Methods section, the compounds shown in Table 1 were synthesized and their total yields were tested. The results are summarized in Table 1.
[0153] Table 1
[0154]
[0155]
[0156]
[0157]
Embodiment 44
[0159] The compounds represented by Formula 1 and Formula 2 were dissolved in a solvent, and the compound synthesized in Table 1 was added as a catalyst. The reaction mixture was stirred at room temperature under nitrogen protection for 12-48 hours. After the reaction was completed, it was filtered, and the filtrate was concentrated under reduced pressure to obtain an oily substance, which was dissolved in ethyl acetate. The organic layer was washed with saturated sodium bicarbonate solution, dried, filtered, and the filtrate was concentrated under reduced pressure to obtain a crude product. The crude product is purified by column chromatography to obtain the target product, which is 3 shown in formula 3. The reaction equation is:
[0160]
[0161] The compounds synthesized in Examples 1-43 were used to implement the above-mentioned synthesis reaction, and the yield and the optical purity (ee%) of the product were determined respectively. The results are summarized in Table 2.
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Abstract
The invention relates to a novel compound, a novel catalyst, a method utilizing the catalyst to synthesize boric acid ester derivatives, a reactor for reaction utilizing the catalyst to synthesize the boric acid ester derivatives and a system utilizing the catalyst to synthesize the boric acid ester derivatives, wherein the novel compound is represented by a formula I. The catalyst can be utilized to effectively catalyze and synthesize the boric acid ester derivatives.
Description
Technical field [0001] The invention relates to the field of medicine and chemical industry. Specifically, the present invention relates to catalysts and their applications. More specifically, the present invention relates to a novel compound, a novel catalyst, a method for synthesizing borate derivatives using the catalyst, a reactor for synthesizing borate derivatives using the catalyst, and a system for synthesizing borate derivatives using the catalyst . Background technique [0002] N-heterocyclic carbene compounds (NHC) are analogues of organic phosphine ligands. Compared with traditional phosphine-metal complexes, NHC metal complexes have many advantages. For example: NHC-metal complexes are stable to water and air, the carbene carbon-metal bond has a large bond energy, and it is not easy to dissociate under heating conditions. Since NHC has stronger electron donating ability than phosphine, it is easy to increase the electron density of the central metal, thereby promo...
Claims
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