Method for preparing indole or indazole compound
A compound and alkyl technology, applied in the field of preparing pharmaceutical indole or indazole compounds, can solve the problems of difficulty in stable scale amplification and lower yield, and achieve the effect of reducing the generation of impurities
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[0083] The preparation method of the present invention may comprise the following steps after forming the intermediate of the above formula 1: replacing the compound represented by the above formula 1 to prepare the compound represented by the following formula 4; reducing the compound represented by the formula 4 to prepare the compound represented by the formula 4 a compound represented by Formula 5; and reacting the compound represented by Formula 5 with a ketone or an aldehyde to prepare a compound represented by Formula 2 above.
[0084] [Formula 4]
[0085]
[0086] [Formula 5]
[0087]
[0088] In the above formula 4 and formula 5, n, m, X, A, R 1 , R 2 , R 3 and R 4 Same as defined above.
[0089] Hereinafter, embodiments of the present invention will be described in more detail so that those of ordinary skill in the art can easily practice the present invention. However, this invention may be embodied in different forms and should not be construed as limit...
Embodiment
[0091] Step a) Synthesis of 4-((7-nitro-2-phenyl-1H-indol-5-yl)methyl)thiomorpholine 1,1-dioxide
[0092] 5-(Hydroxymethyl)-7-nitro-2-phenyl-1H-indole (4.6 kg) and THF (46 L) were added to the reactor and stirred at room temperature, the reactor was cooled to a temperature of 0 °C , then add PBr 3 (2.8 kg) while maintaining the internal temperature of the reaction below 20°C. After the addition was complete, the temperature of the reactor was raised to 25°C, the mixture was stirred for 1 hour, and after analysis of the reaction mixture by sampling showed 5-(hydroxymethyl)-7-nitro-2-phenyl-1H - When the peak of indole is 1.0% or less, the reaction is terminated.
[0093] The completion of the reaction was confirmed, and the reaction mixture was cooled to 0° C., 1,1-diketothiomorpholine hydrochloride (4.4 kg) and N,N-diisopropylethylamine (DIPEA) (8.0 kg ), while maintaining the internal temperature of the reaction below 20°C. After the addition was complete, the temperatu...
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