反应详情

Sodium hydride (13.4 g, 60% dispersion in mineral oil) was added portionwise to (5-chloro-1,3-benzodioxol-4-yl)amine (11.5 g, prepared as described in WO2001094341) in DMA (100 ml) at 0° C. 2,4-Dichloropyrimidine (10 g) was added and the reaction warmed to room temperature and stirred overnight. The reaction was quenched cautiously with water, the solution filtered and concentrated and the residue dissolved in DCM, washed with water and brine, dried and concentrated to give 2-chloro-N-(5-chlorobenzo[d][1,3]dioxol-4-yl)pyrimidin-4-amine as a dark brown oil that was used without further purification (16 g, 85%); NMR Spectrum (300 MHz, DMSO) 6.10 (s, 2H), 6.58 (d, 1H), 6.94 (d, 1H), 7.05 (d, 1H), 8.15 (d, 1H), 9.76 (s, 1H); Mass Spectrum M+ 284.

1. customThe reaction was quenched cautiously with water
2. filtrationthe solution filtered
3. concentrationconcentrated
4. dissolutionthe residue dissolved in DCM
5. washwashed with water and brine
6. customdried
7. concentrationconcentrated