反应详情

温度

140 °C

A mixture of 2-chloroadenosine (0.30 g) and 2-(1-cyclohexenyl)-ethylamine (0.63 g) is stirred under nitrogen for 6 hours at 140° C. The solution is concentrated to dryness at reduced pressure; the residue is dissolved in ethanol, treated with propylene oxide (2 ml) and stirred at room temperature for 16 hours. The mixture is concentrated to dryness at reduced pressure and flash chromatographed through a 25×150 mm column of silica gel using methylene chloride and methanol saturated with ammonia (9:1) as eluent. Fractions containing the desired product are combined, concentrated to dryness at reduced pressure; the residue is redissolved in hot ethanol, the solution is decolorized with charcoal and then concentrated to dryness. The residual solid is triturated with ethanol (2 ml) and collected to afford 2-[2-(1-cyclohexenyl)-ethylamino]adenosine, m.p. 135°-38°.

1. concentrationThe solution is concentrated to dryness at reduced pressure
2. dissolutionthe residue is dissolved in ethanol
3. additiontreated with propylene oxide (2 ml)
4. stirringstirred at room temperature for 16 hours
5. concentrationThe mixture is concentrated to dryness at reduced pressure and flash
6. customchromatographed through a 25×150 mm column of silica gel
7. additionFractions containing the desired product
8. concentrationconcentrated to dryness at reduced pressure
9. dissolutionthe residue is redissolved in hot ethanol
10. concentrationconcentrated to dryness
11. customThe residual solid is triturated with ethanol (2 ml)
12. customcollected