反应详情

温度

160 °C

A mixture of 5-(3-chloropropoxy)-2,3-dihydro-1,4-benzodioxin (0.017 mol), N-2-pyrimidinyl-1,3-propanediamine (0.026 mol) and calcium oxide (5 g) in tetrahydrofuran (150 ml) was stirred overnight at 160° C. (pressure vessel). The mixture was cooled, filtered and the filtrate was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /(CH3OH/NH3)95/5). The pure fractions were collected and the solvent was evaporated, yielding 2.66 g N-[3-[(2,3-dihydro-1,4-benzodioxin-5-yl)oxy]propyl]-N'-2-pyrimidinyl-1,3-propanediamine ethanedioate(1:1) (36.0%); mp. 200.2° C. (comp. 8)

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. customthe filtrate was evaporated
4. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /(CH3OH/NH3)95/5)
5. customThe pure fractions were collected
6. customthe solvent was evaporated