反应详情

To a slurry of 4.0 g. (0.03 mol.) of anhydrous aluminum chloride in 30 ml. of carbon disulfide under a nitrogen atmosphere at 5° is added a mixture of 2.1 g. (0.01 mol.) of 2-phenylbenzothiophene in 40 ml. of 1:1 carbon disulfide-methylene chloride containing 3.06 g. (0.01 mol.) of 4-(3-diethylaminopropoxy)benzoyl chloride. After addition, the reaction mixture is warmed to ambient temperature and stirred for 16 hours. Dilute aqueous hydrochloric acid is added to the mixture and the layers are separated. The aqueous phase is re-extracted with chloroform and the organic layers are combined and concentrated to give a residue which is treated with ethereal hydrochloric acid and chromatographed on silica gel with methanol-chloroform as eluant to give the title compound as the corresponding hydrochloride salt.

1. additiona mixture of 2.1 g
2. additionAfter addition
3. customthe layers are separated
4. extractionThe aqueous phase is re-extracted with chloroform
5. concentrationconcentrated
6. customto give a residue which
7. customchromatographed on silica gel with methanol-chloroform as eluant