In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 29908-11-0, name is (1,4-Dioxan-2-yl)methanol, the common compound, a new synthetic route is introduced below. Formula: C5H10O3
[0284] An oven dried multineck round bottom flask equipped with a condenser and an inlet septum under N2 is loaded with NaH (1.25 equiv., 60% in mineral oil) and dry THF (2.67 mL/mmol). An alcohol (1.2 equiv.) is added dropwise and the resulting mixture is stirred at room temperature for 20 min and subsequently heated at 50 C for 20 min. Then 4-chloro-6,7-dihydrobenzo[a]quinolizin-2-one derivative is added (1.0 equiv.) as a dry solid to the alkoxide mixture (any material that can not be transferred as such is dissolved in dry THF (1.3 mL/mmol) and added to the mixture). The mixture is briefly purged with N2 and heated at 70 C until all starting material is consumed. The mixture is cooled down to room temperature and quenched with saturated aq. NaHCO3. The mixture is then concentrated in vacuo and partitioned between DCM and brine. The aqueous layer is extracted once with DCM and combined organics are dried over Na2SO4 and concentrated to dryness. The crude product is dissolved in MeCN and refluxed for 15 min. The mixture is cooled down to room temperature and the precipitate is separated by filtration. The precipitate is discarded and the filtrate is washed with pentane. The MeCN phase is concentrated to dryness affording the desired product.
The synthetic route of 29908-11-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GALAPAGOS NV; MENET, Christel, Jeanne, Marie; DOYON, Julien, Georges, Pierre-Olivier; CLAES, Pieter, Isabelle, Roger; ALLART, Brigitte; DE WACHTER, Maxim, Maria, Paul; TRICARICO, Giovanni, Alessandro; (168 pag.)WO2016/169911; (2016); A1;,
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