65854-72-0Relevant academic research and scientific papers
Preparation method of stable isotope labeled oxazepam internal standard reagent
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Paragraph 0048-0050, (2021/10/27)
The invention relates to a preparation method of a stable isotope labeled oxazepam internal standard reagent for monitoring the blood concentration of clinical treatment drugs, and belongs to the field of research and development of standard substances for monitoring clinical treatment drugs. The stable isotope labeled oxazepam is obtained by taking stable isotope labeled phenylboronic acid as a raw material through catalytic addition, acylation, cyclization, acetylation, hydrolysis and final separation and purification. The process has the advantages that raw materials needed for synthesis are simple and easy to obtain, reaction conditions are mild, the chemical purity of the target product stable isotope labeled oxazepam can reach 98% or above, the isotope abundance can reach 98% or above, and the preparation method can meet the technical requirements of a stable isotope labeled internal standard reagent needed by a clinical drug monitoring liquid chromatography-tandem mass spectrometry method.
Preparation method of stable isotope labeled alprazolam and estazolam internal standard reagent
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Paragraph 0058-0060, (2021/10/27)
The invention relates to a preparation method of a stable isotope labeled alprazolam and estazolam internal standard reagent for monitoring the blood concentration of a clinical treatment drug, and belongs to a standard substance for monitoring the clinical treatment drug. The stable isotope labeled alprazolam or stable isotope labeled estazolam is obtained by taking stable isotope labeled phenylboronic acid as a raw material, performing catalytic addition, acylation, cyclization, sulfur-oxygen exchange and cyclization and finally conducting separating and purifying. The process has the advantages that raw materials needed for synthesis are simple and easy to obtain, reaction conditions are mild, the chemical purity of the target product stable isotope labeled alprazolam and stable isotope labeled estazolam can reach 98% or above, and the isotope abundance can reach 98% or above. The preparation method can meet the technical requirements of a stable isotope labeling internal standard reagent required by a liquid chromatography-tandem mass spectrometry method for monitoring the blood concentration of a clinical treatment drug.
Intermediate for preparing diazepam-D5 and diazepam-D8 and preparation method of intermediate
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Paragraph 0038; 0039; 0040; 0041, (2018/01/11)
The invention discloses an intermediate for preparing diazepam-D5 and diazepam-D8 and a preparation method of the intermediate. The preparation method comprises the steps: reacting 6-chloro-2-methyl-4H-3,1-benzoxazin-4-one as a raw material with a deuterated bromobenzene Grignard reagent, and carrying out hydrolysis, acylation, cyclization, separation and purification to obtain the intermediate, namely 7-chloro-1,3-dihydro-5-(phenyl-d5)-2H-1,4-benzodiazepin-2-one, for preparing diazepam-D5 and diazepam-D8. The process disclosed by the invention has the characteristics of mild reaction condition, simplicity in operation and the like; and the deuterated diazepam intermediate prepared by using the preparation method is high in chemical purity, high in product quality and good in stability, can be used for preparing standard products of diazepam-D5 and can also be used for preparing standard products of diazepam-D8 and other relevant deuterated standard products.
Diazepam-D5 preparation method
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Paragraph 0037; 0038; 0039; 0040, (2017/12/14)
The invention discloses a diazepam-D5 preparation method. According to the method, 6-chlorine-2-methyl-4H-3, 1-benzoxazine-4-ketone (a compound as shown in a formula) serves as a raw material, and the 6-chlorine-2-methyl-4H-3, 1-benzoxazine-4-ketone and deuterated bromobenzene reagents are reacted, hydrolyzed, acylated, cyclized, methylated, separated and purified to obtain diazepam-D5. The preparation method has the advantages of mild reaction condition, simple in operation and the like, and a diazepam-D5 standard product prepared by the method is high in chemical purity and good in quality and stability and can be conveniently used for analyzing preparation of standard products. The preparation method can be used for producing deuterated internal standard substances when the diazepam-D5 is analyzed and detected.
Diazepam-D8 and preparation method thereof
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Paragraph 0040-0043, (2018/04/01)
The invention discloses diazepam-D8 and a preparation method thereof. The deuterated diazepam D8 is prepared by reacting 6-chloro-2-methyl-4H-3,1-benzoxazine-4-one (a compound shown as a formula I) serving as a raw material with a deuterated bromobenzene Grignard reagent, and performing hydrolysis, acylation, cyclization, methylation, separation and purification. The process disclosed by the invention has the advantages of mild reaction conditions, simple operation and the like. The deuterated diazepam D8 standard prepared by the method has high chemical purity, good product quality and good stability, and can be conveniently used for the preparation of analytical standards. The preparation method disclosed by the invention can be used for producing a deuterated internal standard substance during analysis and direction of diazepam.
DEUTERATED ANALOGS OF ETIFOXINE, THEIR DERIVATIVES AND USES THEROF
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Paragraph 00156, (2016/10/11)
This invention relates to deuterated analogs of etifoxine of Formula 1, solvates, prodrugs, and pharmaceutically acceptable salts thereof, as well as to methods for their preparation and use, and to pharmaceutical compositions. Briefly, this invention is generally directed to deuterated analogs of etifoxine as well as to methods for their preparation and use, and to pharmaceutical compositions containing the same.
