Adding a certain compound to certain chemical reactions, such as: 10485-09-3, name is 2-Bromoindene, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 10485-09-3, Formula: C9H7Br
A 1.45 g (59.8 mmol) piece of magnesium was charged into a sufficiently dried and argon-substituted 200 mL reactor, and stirred vigorously for 30 minutes while heating under reduced pressure. After cooling to room temperature, a reflux condenser was attached, and a piece of iodine and 15 mL of tetrahydrofuran were charged and stirred. A solution of 2.93 g (15.0 mmol) of 2-bromoindene in 15 mL of a diluted solution of tetrahydrofuran is added dropwise (1.0 mL added, followed by heating under reflux with a dryer until the color of iodine disappears, remaining drop after reaction starts) It stirred at room temperature after completion | finish for 2 hours.The reaction solution is diluted with 9.00 mL (75.3 mmol) of dimethylsilyl dichloride in 10 mL of n-hexane diluted solution.The reaction was slowly added at -78 C with cooling, and stirring was continued for 19 hours while returning to room temperature.After distilling off the solvent of the reaction solution and unreacted dimethylsilyl dichloride, 10 mL of tetrahydrofuran and 1.50 mL (16.0 mmol) of 1,3-dimethyl-2-imidazolidinone were added to the residue. In a fully dried, argon purged 100 mL reactor, obtained in Synthesis Example 5-15.62 g (15.0 mmol) of the selected compound (A-5a) and 15 mL of tetrahydrofuran are added, 9.70 mL (hexane solution, 1.55 M, 15.0 mmol) of n-butyllithium solution is added, and the mixture is stirred at room temperature for 2 hours did. The above reaction was cooled to -78 C.The residue was added dropwise to the diluted solution, and stirring was continued for 45 hours while slowly returning to room temperature. Saturated aqueous ammonium chloride solution was added, the extract was extracted with ethyl acetate, and the obtained fraction was washed with saturated brine and dried over anhydrous magnesium sulfate. After filtering the magnesium sulfate, the filtrate is distilled offThe residue thus obtained was purified by silica gel column chromatography to obtain 7.67 g (yield: 94%) of the target product (hereinafter referred to as compound (A-5L)) represented by the following formula (A-5L) It was obtained as a body mixture.
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Reference:
Patent; Mitsui Chemicals, Inc.; Prime Polymer Co., Ltd.; Tanaka, Yoichi; Harada, Yasuyuki; Tamura, Naoya; Hato, Ikki; Tsuchitani, Hiroko; (68 pag.)JP2019/59723; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary