反应详情

Disodium 2,3-dimethyl-1,3-bis(4-sulphonatobutyl)-3H-indolium-5-sulphonate, crude (1.0 g) and malonaldehyde bis(phenyl)mine) HCl (1.0 g) and acetic acid (10 ml) were heated under nitrogen at 130° C. for 10 hrs to give a dark orange-red solution. The solvent was then evaporated under vacuum; the residue was partitioned in a water/dichloromethane/methanol mixture. UV/Vis analysis (ethanol) confirmed the presence of the product in the upper, aqueous layer (λmax=524 nm) while the malonaldehyde starting material was present mainly in the lower, organic layer (λmax=384 nm). The aqueous layer was evaporated under vacuum and purified by HPLC (water/0.1% TFA and acetonitrile/0.1% TFA eluants). Fractions containing the product were pooled and evaporated, freeze-dried from aqueous solution, with final drying under high vacuum over phosphorus pentoxide to give the title product. Yield 240 mg as a red foam.

1. customto give a dark orange-red solution
2. customThe solvent was then evaporated under vacuum
3. customthe residue was partitioned in a water/dichloromethane/methanol mixture
4. customThe aqueous layer was evaporated under vacuum
5. custompurified by HPLC (water/0.1% TFA and acetonitrile/0.1% TFA eluants)
6. additionFractions containing the product
7. customevaporated
8. customfreeze-dried from aqueous solution
9. dry with materialwith final drying under high vacuum over phosphorus pentoxide