Application of 330786-24-8, 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 330786-24-8 as follows.
Under nitrogen protection, Ph3P (29.2g, 112mmol), (3S)-hydroxy-1-tert-butoxycarbonylpiperidine (18.0g, 89.3mmol) was dissolved in 150ml of tetrahydrofuran, cooled to 0 C, the control temperature did not exceed A solution of DIAD (25.3 g, 125 mmol) in tetrahydrofuran (40 ml) was added at 5 C over 20-30 min. Then at 0~5CA solution of 4-amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidine (28.4 g, 93.8 mmol) in tetrahydrofuran (150 ml) was added, Stir at room temperature for 5 h. Add 3.2 ml of water, then add zinc chloride (18.2 g, 134 mmol), stir to warm to 30-40 C for 2.5 h, cool to 0 C ~ 5, filter, and wash with tetrahydrofuran (50 ml ¡Á 2), remove the solvent by rotary evaporation The residual oil was slurried with ethyl acetate (300 ml), hexane (50 ml) was added, filtered, and the residue was washed with ethyl acetate (30 ml ¡Á 2), and the filtrate was water (100ml ¡Á 2), saturated brine (150ml) The organic layer was washed with anhydrous sodium sulfate, and the solvent was evaporated to remove the solvent. The residue was purified by the solvent. The content of Ph3PO was 3.81% (Comparative MgCl2: 32.4% by weight), and isopropanol (40 ml) was added to the residue to warm. Stirring at 50-60 C, cooling the crystals, filtering a small amount of cold isopropanol washing, product: 31.5 g (yield 80.2%), Ph3PO content: 0.28% (compared with MgCl 2 method: yield 85.2%; Ph3PO content: 14 wt%)
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,330786-24-8, its application will become more common.
Reference:
Patent; Fujian Microbiology Institute; Zhao Xueqing; Cheng Jiawei; Lin Yanqin; Fan Lin; Chen Zhong; Xu Minhua; Yi Mingyan; (8 pag.)CN109232581; (2019); A;,
Pyrimidine | C4H4N2 – PubChem,
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