* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Reference：
[1] Journal of the American Chemical Society, 1957, vol. 79, p. 3559
[2] Patent: DE951629, 1953, ,
[3] Patent: CN108409543, 2018, A, . Location in patent: Paragraph 0024; 0025; 0026; 0028
With hydrogenchloride; amalgamated zinc; acetic acid
With triethylsilane; trifluoroacetic acid for 4h; Inert atmosphere; Reflux;
Preparation of 7-chloro-4-hydroxy-2,3-dihydroindene A
Under the protection of nitrogen,To compound C (83 g, 0.45 mol)Triethylsilane added to a solution of trifluoroacetic acid (300 mL)(160 g, 1.38 mol).The reaction solution was then stirred at reflux temperature for 4 hours.After the reaction solution is removed under reduced pressure,The resulting residue was poured into aq. NaOH (2N, 1 L).It was extracted 3 times with hexane (300 mL x 3). The aqueous layer was acidified to pH = 1 with concentrated hydrochloric acid.It was extracted 3 times with ethyl acetate (300 mL x 3). Combine the organic layers,It was washed with water and dried over anhydrous Na 2 SO 4 .After the organic layer is concentrated under reduced pressure, the solvent is evaporated.The residue obtained is crystallized from petroleum ether (b.p. 90-120 ° C).Compound A 53g was obtained,Yield 69%,It is a white solid.
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