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The preparation method of high quality s-2-chlorobutanol

A chlorobutanol, high-quality technology, applied in the field of preparation of high-quality S-2-chlorobutanol, can solve the problems of difficult product guarantee, poor process stability, low quality standards, etc., achieves high optical rotation value, Stable process and good repeatability

Active Publication Date: 2017-06-20
上海弗凯生物科技有限公司
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Problems solved by technology

[0002] L-2-aminobutyric acid is an important pharmaceutical intermediate and chemical raw material, but the current industrial method is still to use chemical method to prepare, the chiral purity is low and the process stability is not good, and the quality standard is relatively low
Using L-2-aminobutyric acid synthesized by the current industrial chemical method as raw material to prepare s-2-chlorobutanol, it is difficult to guarantee high-quality products (EE value reaches 99%)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] L-2-aminobutyric acid prepared by bioreduction

[0013] Replace the resistance and origin of replication of the pET28 vector with the chloramphenicol resistance and origin of replication of pLys S, and then clone threonine deaminase and leucine dehydrogenase into the vector in series; The enzyme and the pcnB gene are connected in series to the pET28a vector; two expression vectors with different resistances are simultaneously transferred into Escherichia coli BL21 (DE3) expression host bacteria, and under the induction of IPTG, the simultaneous expression of the four enzymes is realized.

[0014] The bacterial cells expressing the above four enzymes at the same time were prepared into a suspension, added a certain amount of ammonium formate and threonine, and transformed at 30 degrees, and then continuously added threonine until the final concentration was 0.8 M, L- The conversion of 2-aminobutyric acid basically stops, and the bacterial cells are removed by centrifugat...

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Abstract

The invention relates to a preparation method of high-quality S-2-chlorobutanol. The method comprises the following steps: with L-2-aminobutyric acid prepared by a biological reduction transformation method as a raw material, preparing the S-2-chlorobutanol by adopting a diazotization chlorination method; further esterifying, and reducing with sodium borohydride / titanium tetrachloride, so as to obtain the product. According to the prepared high rotary S-2-chlorobutanol, the EE value is over 99%; and the S-2-chlorobutanol is good in repeatability and stable in process.

Description

technical field [0001] The invention relates to a method for preparing high-quality S-2-chlorobutanol. Background technique [0002] L-2-aminobutyric acid is an important pharmaceutical intermediate and chemical raw material, but the current industrial method is still to use chemical method to prepare, the chiral purity is low, the process stability is not good, and the quality standard is relatively low. Using L-2-aminobutyric acid synthesized by the current industrial chemical method as raw material to prepare s-2-chlorobutanol, it is difficult to guarantee a high-quality product (EE value reaches 99%). Contents of the invention [0003] The object of the present invention is to overcome above-mentioned deficiency, provide a kind of good repeatability, the preparation method of the high-quality S-2-chlorobutanol of process stability. [0004] The purpose of the present invention is achieved like this: [0005] A kind of preparation method of high-quality S-2-chlorobuta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/36C07C29/147C12P13/04C12N15/70C12R1/19
CPCC07C29/147C12P13/04C07C31/36
Inventor 郁庆明
Owner 上海弗凯生物科技有限公司
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