65854-71-9Relevant academic research and scientific papers
Intermediate for preparing diazepam-D5 and diazepam-D8 and preparation method of intermediate
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Paragraph 0034; 0035; 0036; 0037, (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 0033; 0034; 0035; 0036, (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 0036-0039, (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.
