反应详情

13.9 g of 4-bromo-but-1-ene are reacted with 20.2 g of sodium theophylline in 200 ml of dimethyl-formamide at 120° C. with stirring for approximately 6 to 8 hours until the reaction is complete as indicated by thin-layer chromatography. The solvent is then removed under reduced pressure. The residue is dissolved at 20° C. in 100 ml of methylene chloride, separated from insoluble sodium bromide and purified through a column packed with neutral aluminum oxide to remove small quantities of dark-coloured accompanying substances. Melting point: 110° C. (acetone); yield: 21.6 g (91% of theory relative to the starting material used). After thin-layer chromatography on Merck DC finished plates of silica gel 60 F254 with benzene/acetone (6:4) as eluent, the product has an Rf value of 0.54; and with nitromethane/benzene/pyridine (20:10:3) as eluent, an Rf value of 0.65. Utra-violet light was used as indicator, the pyridine of the eluent having, however, to be removed at 50° C. under reduced pressure because of its property to extinguish fluorescence.

1. customThe solvent is then removed under reduced pressure
2. dissolutionThe residue is dissolved at 20° C. in 100 ml of methylene chloride
3. customseparated from insoluble sodium bromide
4. custompurified through a column
5. customto remove small quantities of dark-coloured accompanying substances
6. customhowever, to be removed at 50° C. under reduced pressure because of its property