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A high-performance liquid chromatography method for separating (r), (s)-1-(α-naphthyl) glycidyl ether
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A technology of glycidyl ether and high performance liquid chromatography, applied in the field of high performance liquid chromatography, can solve the problems of chiral chromatography column manufacturing cost, high sales price, short service life, etc.
Active Publication Date: 2022-04-19
云南贝斯泰生物科技有限公司
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However, the manufacturing cost and sales price of the chiral chromatographic column are higher, and the service life is much shorter than that of the conventional C18 chromatographic column
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Embodiment 1
[0025] 1. Instruments and reagents
[0026] 1. Instrument
[0027] 1260 liquid chromatograph (vacuum degasser, binary pump, autosampler) of American Agilent Company.
[0031] The purity of (R)-1-(α-naphthyl)glycidyl ether reference substance and (S)-1-(α-naphthyl)glycidyl ether reference substance is not less than 99%, and the structural formula is as follows figure 1 shown.
[0032] The chiral additive N,N'-bis(tert-butoxycarbonyl)-L-cystine was purchased from McLean's Reagent with a purity of 98%.
[0057] The purity of (R)-1-(α-naphthyl)glycidyl ether reference substance and (S)-1-(α-naphthyl)glycidyl ether reference substance is not less than 99%, and the structural formula is as follows figure 1 shown.
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Abstract
The invention discloses a high performance liquid chromatography method for separating (R) and (S)-1-(α-naphthyl) glycidyl ether. (R), (S)‑1‑(α‑naphthyl) glycidyl ether is an important intermediate for the synthesis of β‑receptor blockers such as natopidil and propranolol, and is widely used in medicine and chemical industry areas, but it is difficult to separate the two. The method of the present invention is based on the cheap carbon octadetaph chromatographic column as a means of separation, and can effectively separate (R)-1-(α-naphthyl) glycidyl ether and (S)-1-(S)- 1‑(α‑naphthyl) glycidyl ether is separated, which greatly reduces the separation cost of (R), (S)‑1‑(α‑naphthyl) glycidyl ether.
Description
technical field [0001] The invention belongs to the field of drug analysis, in particular to a high performance liquid chromatography method for separating (R) and (S)-1-(α-naphthyl) glycidyl ether. Background technique [0002] 1-(α-naphthyl) glycidyl ether is an important intermediate for the synthesis of β-receptor blockers such as naftopidil and propranolol, and is widely used in the fields of medicine and chemical industry (natopidil enantiomer Synthetic Process Optimization of Isomers, Journal of Guangdong Pharmaceutical University, 2019). [0003] 1-(α-naphthyl) glycidyl ether has a chiral center and a pair of enantiomers, namely: (R)-1-(α-naphthyl) glycidyl ether, (S)- 1-(α-naphthyl) glycidyl ether, the chemical structure is as follows: [0004] [0005] (R)-1-(α-Naphthyl)glycidyl ether [0006] [0007] (S)-1-(α-naphthyl)glycidyl ether. [0008] When synthesizing target products with different configurations, the required configurations of 1-(α-naphthyl) g...
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