Triethylamine → HCID 16082226, compound

Participants

Reaction Steps

Into 10 ml of toluene was dissolved 252 mg (0.36 mmol) of 2,2′-bis{di-(3,5-xylyl)phosphinyl}benzophenone, and further 2.0 ml (14.4 mmol) of triethylamine was added thereto, and the resultant solution was cooled to 0° C. Thereto was added 360 μl (3.6 mmol) of trichlorosilane, and then the resultant solution was stirred for 30 minutes while the temperature thereof was kept at 0° C. Thereafter, the temperature thereof was slowly raised to a temperature at which the solution was allowed to be refluxed. The solution was then refluxed for 4 hours. The reaction mixture was cooled, and thereto was dropwise added 10 ml of 25% aqueous sodium hydroxide slowly. The aqueous phase was extracted with 10 ml of methylene chloride. The organic phases were combined, washed with 1N hydrochloric acid two times and then dried over magnesium sulfate. The resultant was concentrated under reduced pressure to distill off the solvent, and then purified by column chromatography on silica gel (ethyl acetate:hexane=1:6) to give 47.7 mg (yield: 20%) of the title compound in the form of a yellow solid.

Provenance & Evidence