反应详情

温度

100 °C

To a stirred solution of triethyl 1,3,5-triazine-2,4,6-tricarboxylate (J. Org. Chem. 59, 4950, 1994) (2.02 g, 6.80 mmol.) in DMF (15 mL) is added 1-aminoethaniminium chloride (1.29 g, 13.60 mmol). After the addition, the mixture is heated at 100° C. for 18 hours then the mixture is extracted three times with ethyl acetate. The combined organic layers are washed with water and brine then is dried over magnesium sulfate. The solvent is removed under reduced pressure and the residue is purified by flash chromatography (heptane/ethyl acetate=3:1) to give diethyl 6-aminopyrimidine-2,4-dicarboxylate; HPLC Retention time 0.89 minutes (condition C); MS 240.3 (M+1).

1. additionAfter the addition
2. extractionthe mixture is extracted three times with ethyl acetate
3. washThe combined organic layers are washed with water and brine
4. dry with materialthen is dried over magnesium sulfate
5. customThe solvent is removed under reduced pressure
6. customthe residue is purified by flash chromatography (heptane/ethyl acetate=3:1)