反应详情

温度

50 °C

2.53 g of anhydrous potassium carbonate are added to a solution of 2.5 g of 3,6-diaminoacridine hydrochloride and 2.95 g of 1-eicosyl bromide in 20 ml of N,N'-dimethylethyleneurea, and the mixture is stirred at 50° C. for 86 hours. The cooled reaction mixture is subsequently poured into water, and the orange-brown suspension is extracted with methylene chloride. The organic phase is washed with water and dried over sodium sulfate. After evaporation, 2N HCl is added to the brown oil. The red precipitate formed is filtered off, washed with water and then dried in a high vacuum. The resultant red-brown crystals are taken up in methylene chloride/methanol (10:1) and chromatographed on silica gel. After evaporation, the residue is taken up in diethyl ether/methanol (10:1) and re-chromatographed on silica gel, giving the title compound as red crystals, absorption spectrum (ethanol): λmax =472 nm; ε=42 200.

1. customThe cooled reaction mixture
2. extractionthe orange-brown suspension is extracted with methylene chloride
3. washThe organic phase is washed with water
4. dry with materialdried over sodium sulfate
5. customAfter evaporation, 2N HCl
6. additionis added to the brown oil
7. customThe red precipitate formed
8. filtrationis filtered off
9. washwashed with water
10. customdried in a high vacuum
11. customchromatographed on silica gel
12. customAfter evaporation
13. customre-chromatographed on silica gel
14. customgiving
15. customthe title compound as red crystals, absorption spectrum (ethanol)