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抗生素中间体中合成过程检测方案(化学合成仪)

检测样品 化药新药研发

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连续流动合成(也可称为微型合成)在有机合成中应用非常广泛,尤其在化学合成药物中间体的合成中,更加方便。该方法介绍连续流动方式合成Zyvox中间体的过程。

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FlowSynTM Application Note 8:Scale-up Synthesis of a ZyvoxTM Intermediate Objective: ZyvoxTM (Upjohn) was the first example of a new class of oxazolidinone antibiotics that are activeagainst MRSA. In this example, the scale-up abilities of FlowSynTM are demonstrated byperforming the first step in a possible synthesis of this compound on a 100 g scale. Method: System solvent: Dimethylformamide.Stock solution A: 2.0 M 3,4-Difluoronitrobenzene 1 (55.0 mL, 0.50 mol) in DMF (195 mL). Stock solution B: 4.0 M Morpholine 2 (87.0g, 0.75 mol) in DMF (163 mL). A 45 psi fixed back-pressure regulator was fitted and used in all experiments. Flow Scale-up using Start Experiment'Interface FlowSynTM is equipped with a program that allows unattended operation and is able to run a flowexperiment automatically, stopping and cleaning the instrument when the reaction is complete. 1.FlowSynTM was fitted with a 20 mL SS tubing reactor cassette, and the heating unit wastensioned to ensure optimal thermal contact. 2.A 40 psi fixed BPR was connected in-line to the outflow from the tubing reactor before thecollection valve 3.The Collect'outflow from the collection valve was directed into a 5 L Duran collection bottlecontaining water (4 L) mounted on a stirrer. 4.The selection valves were set to 'Reagent' and the reagent lines were primed up to the valves. 5.The selection valves were set to `Solvent' and the solvent lines were primed. 6.The pumps were started at 4.0 mL/min to rapidly prime the system with solvent and remove allair bubbles (indicated by a stable pressure reading). The pumps were calibrated at 1.00 mL/minas previously [no further adjustments were necessary]. 7.The following flow parameters were entered into the 'Setup Experiment' screen. Reactors: Coil Reaction Time: 8.00 min (00:08:00) Coil Type: User Total Flow Rate: 2.50 mL/min Coil Volume: 20 mL Volume A: 225 mL (0.45 mol) Coil Temp:100°CVolume B:225 mLCol. Temp.0°CA:B Ratio:1.0:1.0 Pressure: Auto Post Collect: 25.0 mL Inlet A: RPost Wa sh: 20.0 mLR Inlet B: Reaction time = 3.00 h. 8.Upon pressing `Run Experiment', FlowSynTM equilibrates to the set temperature and then runsthe flow experiment, before finally cleaning the system by flushing with system solvent (`PostWash'). 9.The precipitated reaction product was collected by filtration, washed with water (3 x 100 mL),then air-dried before drying o/n @ 50°C in vacuo to afford the nitro-aniline 3 as a free-flowingyellow powder (101 g, 99%): m.p.=113-115℃ Throughput = 0.15 mol/h (34 g/h). 'H NMR (CDCl3, 400 MHz): 8-7.20-7.30 (m, 8H), 7.10-7.15 (m, 2H), 6.70 (s, 1H). Supplementary Information: Figure 2. Schematic FlowSynTM configuration used. -- --

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博盛技术(中国)有限公司为您提供《抗生素中间体中合成过程检测方案(化学合成仪)》,该方案主要用于化药新药研发中其他检测,参考标准《暂无》,《抗生素中间体中合成过程检测方案(化学合成仪)》用到的仪器有流动合成系统。

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