反应详情

A solution of 8 g of 4,6-dichloro-5-pyrimidinamine, and 7 g of 1H-indol-1-amine, in 100 ml N-methyl-2-pyrrolidone was stirred at 130°-135° for seven hours, then cooled, stirred with water and extracted with ether. The organic extract was washed with water and saturated sodium chloride, dried (anhy. MgSO4), filtered and evaporated to 16 g of a residue. This was purified by flash chromatography (silica, 5% ethyl acetate/DCM) to give 10 g solid. This was combined with product obtained from other condensations and purified by HPLC (silica 5% ethyl acetate/DCM) to give 7 g oil. This oil was crystallized from ether-petroleum ether to give 2.2 g solid, 6-Chloro-N4 -(1H-indol-1-yl)-4,5-pyrimidinediamine, m.p. 175°-176°C.

1. temperaturecooled
2. extractionextracted with ether
3. extractionThe organic extract
4. washwas washed with water and saturated sodium chloride
5. dry with materialdried (anhy. MgSO4)
6. filtrationfiltered
7. customevaporated to 16 g of a residue
8. customThis was purified by flash chromatography (silica, 5% ethyl acetate/DCM)