反应详情

温度

150 °C

A mixture of (6-chloro-pyrimidin-4-yl)-methyl-amine (Example 1) (750 mg, 5.2 mmol), 3-dimethylaminomethyl-phenylamine (787 mg, 5.2 mmol) and 4N HCl in dioxane (15 ml) is heated in a sealed tube to 150° C. for 5 h. The reaction mixture is concentrated, diluted with DCM and a saturated aqueous solution of sodium bicarbonate. The aqueous layer is separated and extracted with DCM. The organic phase is washed with brine, dried (sodium sulfate), filtered and concentrated. Purification of the residue by silica gel column chromatography (DCM/MeOH+1% NH3aq, 9:1) affords 800 mg of the title compound as a white solid: ESI-MS: 258.1 [MH]+; tR=1.00 min (purity: 100%, gradient J); TLC: Rf=0.14 (DCM/MeOH+1% NH3aq, 9:1).

1. concentrationThe reaction mixture is concentrated
2. additiondiluted with DCM
3. customThe aqueous layer is separated
4. extractionextracted with DCM
5. washThe organic phase is washed with brine
6. dry with materialdried (sodium sulfate)
7. filtrationfiltered
8. concentrationconcentrated
9. customPurification of the residue by silica gel column chromatography (DCM/MeOH+1% NH3aq, 9:1)