By the way, if you are interested in learning more fun chemistry with your kids, get your hands into one chemistry set now, and start enjoying the best part of chemistry: experiments about 1-((2S,3S)-2-(Benzyloxy)pentan-3-yl)-4-(4-(4-(4-hydroxyphenyl)piperazin-1-yl)phenyl)-1H-1,2,4-triazol-5(4H)-one.
Reference of 184177-83-1, New discoveries in chemical research and development in 2021. We’ll be discussing some of the latest developments in chemical about CAS: 184177-83-1, name is 1-((2S,3S)-2-(Benzyloxy)pentan-3-yl)-4-(4-(4-(4-hydroxyphenyl)piperazin-1-yl)phenyl)-1H-1,2,4-triazol-5(4H)-one, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
The 35.01 kg dimethyl sulfoxide, the mass concentration is 50% aqueous sodium hydroxide solution (sodium hydroxide 1.24 kg dissolved in pure water 1.24 kg, the mass concentration of the refer to sodium hydroxide of the quality of the sodium hydroxide solution the percentage of the total mass of the), adding 50L glass in the reactor, stirring solution cleaning, then adding 5.31 kg compound (III), stirring 20 – 30 minutes, adding 4.60 kg (3S, 5R) – toluene -4 – sulfonic acid 5 – (2, 4 – difluorophenyl) -5 – (1H – 1, 2, 4 – triazole -1 – yl) methyl tetrahydrofuran -3 – yl methyl ester (IV). After the completion of the feeding, temperature control 25 ± 5 C reaction 8 – 12 hours. TLC monitoring reaction, after the reaction. Control the temperature 20 – 30 C, the reaction with the sampler to 53.05 kg purification of water 100L glass reactor (rotational speed 200 – 300 rpm, dropping time 0.5 – 1.0 hours), continuously stirred for 0.5 – 1 hour. Centrifugal then adding to the basic solvent-free outflow; cake purified water 10.61 kg rear plate the basic solvent-free centrifugal to flow out. The centrifugal solid all input 50L glass in the reactor, adding 23.79 kg ethyl acetate, stirring until the solid completely dissolved. Layered, collecting the upper organic phase. Add silica gel 1.06 kg, heating to 50 – 60 C stirring 0.5 – 1 hour, cooled to 15 – 25 C, filtering. The filtrate batch transfer to 20L in the rotary evaporating bottle, at the vacuum degree of – 0.08 – – 0.1 mpa lower, control temperature 50 ± 10 C, concentrated to remove the ethyl acetate, to the solvent-free steam. To obtain brown oily matter. The oil of transfer to the 50L glass in the reactor, adding ethyl acetate 23.79 kg, heating to 50 ± 5 C, adds by drops positively hexane 36.71 kg (the dropping time 0.5 – 1.0 hours). Lowering the temperature to 20 ± 5 C stirring 2 – 3 hours, centrifugal to the solvent-free outflow, filter cake using mixed solvent (ethyl acetate 4.76 kg hexane 7.34 kg) leaching, centrifugal then adding to the solvent-free outflow. The centrifugal throughout the batch of wet product at the vacuum degree of – 0.08 – – 0.1 mpa lower, control temperature 40 – 50 C decompression drying 6 – 10 hours. A gray solid 6.00 kg compound (II). HPLC purity: 96.1%, yield: 73.4%.
By the way, if you are interested in learning more fun chemistry with your kids, get your hands into one chemistry set now, and start enjoying the best part of chemistry: experiments about 1-((2S,3S)-2-(Benzyloxy)pentan-3-yl)-4-(4-(4-(4-hydroxyphenyl)piperazin-1-yl)phenyl)-1H-1,2,4-triazol-5(4H)-one.
Reference:
Patent; Shanghai Bozhi Yan Xin Pharmaceutical Co., Ltd.; Ying Shuhuan; Pi Hongjun; Liu Zhenfeng; Chen Jian; Qiao Yanhe; (12 pag.)CN106749207; (2017); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics