6283-04-1Relevant articles and documents
Rhodium-Catalyzed Addition of Organozinc Iodides to Carbon-11 Isocyanates
Fouad, Moustafa H.,Ismailani, Uzair S.,Mair, Braeden A.,Munch, Maxime,Rotstein, Benjamin H.
supporting information, p. 2746 - 2750 (2020/04/16)
Amides were prepared using rhodium-catalyzed coupling of organozinc iodides and carbon-11 (11C, t1/2 = 20.4 min) isocyanates. Nonradioactive isocyanates and sp3 or sp2 organozinc iodides generated amides in yields of 13%-87%. Incorporation of cyclotron-produced [11C]CO2 into 11C-amide products proceeded in yields of 5%-99%. The synthetic utility of the methodology was demonstrated through the isolation of [11C]N-(4-fluorophenyl)-4-methoxybenzamide ([11C]6g) with a molar activity of 267 GBq μmol-1 and 12% radiochemical yield in 21 min from the beginning of synthesis.
Flow-based enzymatic synthesis of melatonin and other high value tryptamine derivatives: A five-minute intensified process
Contente, Martina Letizia,Farris, Stefano,Tamborini, Lucia,Molinari, Francesco,Paradisi, Francesca
supporting information, p. 3263 - 3266 (2019/06/24)
To increase the uptake of biocatalytic processes by industry, it is essential to demonstrate the reliability of enzyme-based methodologies directly applied to the production of high value products. Here, a unique, efficient, and sustainable enzymatic platform for the multi-gram synthesis of melatonin, projected to generate around 1.5 billion U.S. dollars worldwide by 2021, and its analogues was developed. The system exploits the covalent immobilization of MsAcT (transferase from Mycobacterium smegmatis) onto agarose beads increasing the robustness and longevity of the immobilized biocatalyst. The fully-automated process deriving from the integration between biocatalysis and flow chemistry is designed to maximize the overall yields (58-92%) and reduce reaction times (5 min), overcoming the limitation often associated with bioprocesses and bridging the gap between lab scale and industrial production.
Production preparation method of p-nitrophenylethylamine hydrochloride
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Paragraph 0070, (2018/03/23)
The invention provides a production preparation method of p-nitrophenylethylamine hydrochloride, belongs to the technical field of drug synthesis, and solves the problems that in the prior art the synthetic p-nitrophenylethylamine hydrochloride is low in conversion rate of and is not suitable for large-scale industrial production. Synthesis steps include 1) amino protection, to be more specific, using beta-phenylethylamine as a raw material for reacting with an acyl protecting agent in a solvent to obtain an intermediate 1; 2) nitrating reaction, to be more specific, adding dropwise the intermediate 1 prepared by the step 1) into concentrated sulfuric acid, maintaining reaction temperature at room temperature, slowly adding dropwise concentrated nitric acid, after the completion of the reaction, adding crushed ice, adding an alkaline solution to adjust the pH to alkaline, and filtering to obtain an intermediate 2; and 3) deprotection, to be more specific, adding dropwise hydrochloric acid into the intermediate 2 in a solvent to adjust the pH to acid, heating to reflux, cooling, and precipitating the product p-nitrophenylethylamine hydrochloride. The production preparation method ofthe p-nitrophenylethylamine hydrochloride has low cost and high product yield, and is suitable for large-scale industrial production.
