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ChemicalBook CAS DataBase List spiro-(adamantane-2,9'-fluorene)
727730-31-6

spiro-(adamantane-2,9'-fluorene) synthesis

7synthesis methods
Tricyclo[3.3.1.13,7]decan-2-ol, 2-[1,1'-biphenyl]-2-yl-

727730-30-5
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spiro-(adamantane-2,9'-fluorene)

727730-31-6
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Yield:727730-31-6 99.7%

Reaction Conditions:

with trifluoroacetic acid in dichloromethane; for 2 h;Inert atmosphere;

Steps:



Add intermediate I-M-1 (27.06 g, 88.97 mmol), trifluoroacetic acid (46.90 g, 483.36 mmol) and dichloromethane (300 mL) to a round bottom flask, and stir for 2 hours under nitrogen protection;Then, an aqueous solution of sodium hydroxide was added to the reaction solution to pH = 8, and the liquid phase was separated. The organic phase was dried using anhydrous magnesium sulfate, filtered, and the solvent was removed under reduced pressure. Purification by silica gel column chromatography gave Intermediate IM-2 as a white solid (25.40 g, yield: 99.70%).

References:

CN110615759,2019,A Location in patent:Paragraph 0165; 0166