反应详情

A solution of 2-diethylaminoethyl chloride [obtained from 12.9 g (0.075 mole) of 2-diethylaminoethyl chloride hydrochloride] in 100 ml of toluene (dried over molecular sieves) is added to a mixture of 4.9 g (0.025 mole) of 2,7-dihydroxyfluorene and 2.7 g (0.05 mole) of sodium methoxide in 200 ml of toluene (dried over molecular sieves). This mixture is refluxed with stirring for three hours. Upon cooling the mixture is filtered to remove the precipitated sodium chloride. The toluene solution is washed three times with water, then once with a saturated sodium chloride solution and dried over anhydrous magnesium sulfate. This mixture is filtered and the filtrate acidified to Congo Red with ethereal hydrogen chloride. The solid which precipitates is filtered, dissolved in butanone with enough methanol added to effect solution, decolorized with charcoal, and the product obtained at 80°C under vacuum, 2,7-bis(2-diethylaminoethoxy)fluorene dihydrochloride. M.P. 213°-216°C.

1. temperatureThis mixture is refluxed
2. temperatureUpon cooling the mixture
3. filtrationis filtered
4. customto remove the precipitated sodium chloride
5. washThe toluene solution is washed three times with water
6. dry with materialonce with a saturated sodium chloride solution and dried over anhydrous magnesium sulfate
7. filtrationThis mixture is filtered
8. customThe solid which precipitates
9. filtrationis filtered
10. dissolutiondissolved in butanone with enough methanol
11. additionadded to effect solution