反应详情

温度

120 °C

To a solution of 6-chloropurine (5.0 g, 0.032 mole) in 50 ml 1-methyl-2-pyrrolidinone, was added 1 ml ethereal-HCl; followed by a solution of N-(1H-indol-1-yl)-N-propylamine (5.2 g, 0.030 mole) in 50 ml 1-methyl-2-pyrrolidinone. After stirring at 120° C. for six hours, the mixture was cooled, poured into 500 ml water and stirred for five minutes, pH adjusted to 10 with Na2CO3 ; then extracted with ethyl acetate. The organic layer was washed with water, then dried (saturated NaCl, anhydrous MgSO4). After filtering, the solution was evaporated to an oil, about 8 g, which was eluted on a silica gel column with ethyl acetate via high pressure liquid chromatography. The desired fractions were combined, then evaporated to yield 2.2 g (25%) of N-(1H-indol-1-yl)-N-propyl-9H-purin-6-amine, m.p. 90°-5° C.

1. temperaturethe mixture was cooled
2. stirringstirred for five minutes
3. extractionthen extracted with ethyl acetate
4. washThe organic layer was washed with water
5. dry with materialdried (saturated NaCl, anhydrous MgSO4)
6. filtrationAfter filtering
7. customthe solution was evaporated to an oil, about 8 g, which
8. washwas eluted on a silica gel column with ethyl acetate via high pressure liquid chromatography
9. customevaporated