38560-30-4Relevant articles and documents
Preparation method of apixaban intermediate suitable for industrial production
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Paragraph 0032; 0036; 0038, (2021/08/19)
The invention discloses a synthesis method of an apixaban intermediate suitable for industrial production. The method comprises the following steps: carrying out phase-transfer catalytic amidation reaction on paranitroaniline and 5-chlorovaleryl chloride in an organic phase and water phase two-phase system under an inorganic weakly alkaline condition to obtain an APM01 solution, and adding a sodium hydroxide water solution, and cyclizing in a pot to obtain an APM02 solution; directly carrying out alpha-reactive hydrogen dichlorination on an APM02 organic solution and phosphorus pentachloride after simple acid pickling, liquid separation and drying to obtain an APM03 solution; carrying out condensation-elimination reaction on the APM03 solution and excessive morpholine after simple acid pickling and liquid separation, and carrying out simple crystallization and purification treatment to separate out an APM04 solid, and reducing the APM04 into APM05 by sodium sulfide; and carrying out amidation-cyclization two-step one-pot reaction on the APM05 and 5-chlorovaleryl chloride to prepare a key intermediate APM07. According to the method, the synthesis efficiency of the apixaban intermediate is improved, the reaction is mild, and dangerous NaH and other expensive reagents are not used, so that the production cost is saved, the operation is simple, and the method is suitable for industrial popularization.
Preparation method of apixaban and intermediates thereof
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Paragraph 0121, (2018/05/16)
The invention discloses a preparation method of apixaban and intermediates thereof. The invention provides a preparation method of an apixaban intermediate I. The preparation method of the apixaban intermediate I comprises the step of performing nucleophilic substitution reaction on an apixaban intermediate II and p-fluoronitrobenzene in an organic solvent in the presence of an alkali to obtain the apixaban intermediate I. The preparation method has short steps, simple and safe operation, simple post-treatment steps, environmental friendliness and high total yield, and the obtained product hashigh purity, low production cost and high atomic utilization, and is suitable for industrial production. The formula is shown in the description.
PROCESS FOR THE PREPARATION OF APIXABAN AND INTERMEDIATES THEREOF
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Paragraph 0138; 0139, (2017/06/12)
The present invention refers to novel process for the preparation of Apixaban. Further, the invention also related to a process for the preparation of intermediate of Apixaban from very basic and cheap row material i.e. Aniline which is widely commercially available. The present invention provides process for preparation of Apixaban using a different sequence of synthetic steps and does not involve use of Ullmann reaction.