反应详情

温度

80 °C

A mixture of (4-chloro-[1,3,5]triazin-2-yl)-methyl-amine (290 mg, 2.00 mmol), NaI (28 mg) and 4-(4-ethylpiperazin-1-yl)-aniline (410 mg, 2.0 mmol) in EtOH (20 ml) and N-ethyl-diisopropyl amine (350 μl, 2.0 mmol) is heated to 80° C. for 3 h under a nitrogen atmosphere. The reaction mixture is cooled to RT, concentrated partially in vacuo and diluted with hexane at 0° C. The precipitate is filtered off, washed with Et2O and re-dissolved in EE and water. The separated off aqueous phase is extracted twice with EE, the organic layer washed with water and brine, dried (Na2SO4) and concentrated, yielding the title compound: ESI-MS: 314 [MH]+; TLC: Rf=0.10 (DCM/MeOH 9:1).

1. temperatureThe reaction mixture is cooled to RT
2. concentrationconcentrated partially in vacuo
3. additiondiluted with hexane at 0° C
4. filtrationThe precipitate is filtered off
5. washwashed with Et2O
6. dissolutionre-dissolved in EE and water
7. customThe separated off aqueous phase
8. extractionis extracted twice with EE
9. washthe organic layer washed with water and brine
10. dry with materialdried (Na2SO4)
11. concentrationconcentrated