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 52787-14-1 as follows. COA of Formula: C11H12O4
To a mixture of K2CO3 (1194.5 g), homoterephthalic acid dimethyl ester (600 g) in DMAc (3000 mL), propargyl bromide (582.43 g) was added followed by TBAI (106.41 g) at 25-30 C. and stirred for 20-26 hours. The reaction was monitored by HPLC and found the ratio of Monopropargyl homoterephthalic Acid Dimethyl Ester to that of dipropargyl homoterephthalic Acid Dimethyl Ester to be not less than 85:15. After 26 hours the reaction mixture was quenched with DM water (3000 ml) and extracted with ethyl acetate (2*3000 ml). The organic layer was separated and back-extracted with DM water (3000 ml). The organic layer was then evaporated to dryness at reduced pressure on a rotary evaporator (below 60 C.). Further IPA (1000 ml) was added to the residue and evaporated to dryness at reduced pressure. The crude product was crystallized by dissolving in IPA (000 ml) at 45-50 C. and cooled to 0-5 C. and stirred for 1-2 hours. The product was vacuum filtered. The product obtained was further crystallized with IPA (1800 ml) saturated with Ethyl acetate (54 ml) by dissolving at 55-60 C. and stirred at 20-25 C. for 2-3 hours, followed by stirring at 0-5 C. for 2-3 hours. The solid was filtered and dried under vacuum at 40-45 C. to give 466 g (65.6%) of the title compound. Purity: 99.19%
According to the analysis of related databases, 52787-14-1, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Fresenius Kabi Oncology Limited; Lahiri, Saswata; Gupta, Nitin; Singh, Hemant Kumar; Panda, Nilendu; Handa, Vishal; Abul, Azim; Gupta, Chandan Kumar; Sanghani, Sunil; Sonavane, Ghanashyam Madhukar; US2015/183789; (2015); A1;,
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