反应详情

A mixture of 3-aminomethyl-3-hydroxymethyloxetane (1.17 g, 0.01 mol), 2-amino-4,6-dichloropyrimidine (1.64 g, 0.01 mol), ethanol (40 ml) and triethylamine (4 ml) was refluxed for one day. The solvent was distilled away under reduced pressure and ethyl acetate was added to the residue. The mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=20:1, later 10:1) to give colorless prism crystals (0.8 g, 32.8%), m.p. 185-186° C. (acetone).

1. temperaturewas refluxed for one day
2. distillationThe solvent was distilled away under reduced pressure and ethyl acetate
3. additionwas added to the residue
4. washThe mixture was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled away under reduced pressure
7. customthe residue was purified by silica gel column chromatography (chloroform