Potassium Iodide → 1,1'-(Fluoranthene-3,9-diyl)bis[4-(diethylamino)butan-1-one]--hydrogen chloride (1/2)

反応式

[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:8]=[CH:9][C:10]2[C:11]3[C:16]([C:17]4[C:22]=2[C:21]=1[CH:20]=[CH:19][CH:18]=4)=[CH:15][CH:14]=[C:13]([C:23](=[O:28])[CH2:24][CH2:25][CH2:26]Cl)[CH:12]=3)=[O:6].[CH2:29]([NH:31][CH2:32][CH3:33])[CH3:30].[I-].[K+]>O1CCCC1>[ClH:1].[ClH:1].[CH2:29]([N:31]([CH2:32][CH3:33])[CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:8]=[CH:9][C:10]2[C:11]3[C:16]([C:17]4[C:22]=2[C:21]=1[CH:20]=[CH:19][CH:18]=4)=[CH:15][CH:14]=[C:13]([C:23](=[O:28])[CH2:24][CH2:25][CH2:26][N:31]([CH2:32][CH3:33])[CH2:29][CH3:30])[CH:12]=3)=[O:6])[CH3:30]

参加物

実験手順

A solution of 15.0 g (0.037 mole) of 3,9-bis(4-chlorobutyryl)fluoranthene, 100 ml of diethylamine, 2.0 g of potassium iodide and 100 ml of tetrahydrofuran (THF) is heated at reflux with stirring for 3 days and filtered. The filtrate is poured onto ice water and the oil which separates is decanted and dissolved in ether. The ether solution is washed with a water-saturated sodium chloride solution, dried over magnesium sulfate and filtered. The filtrate is acidified with ethereal HCl, and the resulting precipitate is recrystallized twice from methanol-butanone to yield 3,9-bis(4-diethylaminobutyryl)fluoranthene dihydrochloride. M.P. 236°-239°C.