反应详情

温度

70 °C

2,6-dichloro-3,5-dimethoxyphenylisocyanate (1.25 eq.) is added to a solution of N-(3-dimethylaminomethyl-phenyl)-N′-methyl-pyrimidine-4,6-diamine (93 mg, 0.36 mmol, 1 eq.) in toluene (3 ml), at 70° C. and under an argon atmosphere. The resulting mixture is stirred at 70° C. for 18 h, allowed to cool to RT, and 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 crude product by silica gel column chromatography (DCM/MeOH+1% NH3aq, 9:1) affords 121 mg of the title compound as a white solid: ESI-MS: 504.9/506.9 [MH]+; tR=3.64 min (purity: 100%, gradient J); TLC: Rf=0.12 (DCM/MeOH+1% NH3aq, 9:1).

1. temperatureto cool to RT
2. customThe aqueous layer is separated
3. extractionextracted with DCM
4. washThe organic phase is washed with brine
5. dry with materialdried (sodium sulfate)
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification of the crude product by silica gel column chromatography (DCM/MeOH+1% NH3aq, 9:1)