Synthetic Route of 330786-24-8, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 330786-24-8 as follows.
To 200L reaction kettle adding 124.60 kg tetrahydrofuran, are added under stirring 3 – (4 -)-1H-[34-D]-4-(SM1)(4.00kg1eq)(S)-1-Oxycarbonyl -3 – hydroxy piperidine (SM2) (7.96 kg, 3eq), triphenylphosphine (10.40 kg, 3eq). 25[…] (will be 8.00 kg, 3eq azo-phthalic acid diisopropyl ester soluble in 8.00 kg of in tetrahydrofuran),325(TLCMonitoring: ethyl acetate: methanol=10:1). Stirring under reduced pressure distillation. Temperature control 15 C, dropwise 24.00kg325The reaction is complete (TLC monitoring: dichloromethane: ethyl acetate=5:3). Dichloromethane is used for extraction of the aqueous phase(60.00kg)45.00kgStirring 30 minutes later, the static layering, the minute eliminates upper organic phase. The remaining aqueous phase is added to the 200L anti-1535.00kg 20(9.60Kg sodium hydroxide into 38.40 kg of pure water), the use of pH test paper monitoring reaction solution, pH=5 – 6(2)100LAdding 19.20v ethanol, 0.10 kg of activated carbon, heated to 75 C reflux stirring 2 hours. 1.60kg100LStop heating, water bath cooling, stirring crystallization, when the temperature is reduced to 25 C, thermal crystallization 2 hours. 5.60kg6012Powder 3.75 kg, yield: 85%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,330786-24-8, its application will become more common.
Reference:
Patent; Beijing Rui Chong Kang Tai Pharmaceutical Research Institute Limited; Gu, Huijuan; Chen, Yan; Zhang, Fan; Li, Wei; Liu, Xiangwei; (18 pag.)CN106146512; (2016); A;,
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