65854-72-0Relevant articles and documents
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.
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-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.