Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 145691-59-4, name is (3,5-Dibromophenyl)methanol. A new synthetic method of this compound is introduced below., Recommanded Product: 145691-59-4
Step 2: To a mixture of (3,5-dibromophenyl)methanol (1 g, 3.759 mmol, 1 equiv) and PdCI2(dppf).CH2Cl2 complex (0.21 g, 0.263 mmol, 0.07 equiv) in 10 mL of dry THF at -70 ¡ãC was added 1 M diethyl zinc in hexane (15 mL). The resulting mixture was allowed to warm to room temperature, and stirred at 45 ¡ãC for overnight. To drive the reaction to completion, additional 11.3 mL of 1 M diethyl zinc in hexane was added with continued stirring at 45 ¡ãC for overnight. After cooling, the reaction mixture was added to a stirred mixture of dilute HCI and EtOAc. Organic layer was separated, washed with water, dried over Na2S04, filtered, and concentrated in vacuo to afford crude product. The crude product was purified by flash column chromatography with silica gel cartridge using gradient elution of 0 to 10percent EtOAc in Hexane. The collected fractions with pure product were combined and concentrated in vacuo to afford (3,5-diethylphenyl)methanol as colorless liquid (0.2 g, 32percent). LC-MS (ES) m/z = 147.2 [M+H]+. H NMR (400 MHz, DMSO-d6) delta ppm 1.14 (t, J = 7.2 Hz, 6H), 2.50 – 2.56 (m, 4H), 4.41 (d, J = 5.2 Hz, 2H), 5.01 (t, J = 5.6 Hz, 1 H), 6.87 (s, 1 H), 6.93 (s, 2H).
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Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; AXTEN, Jeffrey Michael; FAUCHER, Nicolas Eric; DAUGAN, Alain Claude-Marie; (153 pag.)WO2017/46739; (2017); A1;,
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