反应详情

温度

150 °C

A mixture of (6-chloro-pyrimidin-4-yl)-methyl-amine (385 mg, 2.68 mmol, 1.1 equiv), 3-(4-methyl-piperazin-1-ylmethyl)-phenylamine (500 mg, 2.44 mmol) and 4N HCl in dioxane (7 mL) is heated in a sealed tube to 150° C. for 17.5 h. The solvent is removed and the residue diluted with DCM and a saturated aqueous solution of NaHCO3. The aqueous layer is separated and extracted with DCM and DCM/MeOH (95:5). The organic phase is washed with brine, dried (Na2SO4), filtered and concentrated. Purification of the residue by silica gel MPLC (DCM/MeOH+1% NH3aq, 95:5) affords the title compound as a beige solid: ESI-MS: 313.2 [MH]+; tR=1.00 min (purity: 100%, system 1); TLC: Rf=0.05 (DCM/MeOH+1% NH3aq, 9:1).

1. customThe solvent is removed
2. additionthe residue diluted with DCM
3. customThe aqueous layer is separated
4. extractionextracted with DCM and DCM/MeOH (95:5)
5. washThe organic phase is washed with brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customPurification of the residue by silica gel MPLC (DCM/MeOH+1% NH3aq, 95:5)