反应详情

0.48 g (20 mmoles) of sodium is dissolved in 20 ml of anhydrous ethanol. This solution is added to an ethanol solution containing 2.48 g (10 mmoles) of N-[imino(cyclopropylamino)methyl]-4-morpholinecarboximidamide hydrochloride, and 2.82 g (22 mmoles) of ethyl 1-methylcyclopropane-carboxylate are then also added to the mixture. The mixture is then heated under reflux under nitrogen for 88 hours. It is cooled, the alcohol is evaporated under reduced pressure and the residue is redissolved in 50 ml of water and 200 ml of dichloromethane. The aqueous phase is separated off and the organic phase is washed twice with 50 ml of water and dried over magnesium sulfate. The solvent is evaporated under reduced pressure and the residue is recrystallized from a 1:1 (v/v) mixture of petroleum ether-dichloromethane. 0.49 g of 2-cyclopropylamino-4-(1-methylcyclopropyl)-6-morpholino-1,3,5-triazine is obtained. Yield: 17%. M.P.: 94°-95°% C.

1. additionare then also added to the mixture
2. temperatureThe mixture is then heated
3. temperatureunder reflux under nitrogen for 88 hours
4. temperatureIt is cooled
5. customthe alcohol is evaporated under reduced pressure
6. dissolutionthe residue is redissolved in 50 ml of water
7. customThe aqueous phase is separated off
8. washthe organic phase is washed twice with 50 ml of water
9. dry with materialdried over magnesium sulfate
10. customThe solvent is evaporated under reduced pressure
11. customthe residue is recrystallized from a 1:1 (v/v) mixture of petroleum ether-dichloromethane