反应详情

温度

100 °C

A solution of 2-chloro-N-(2,2-diphenylethyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (Preparation 20) (49.7 g, 0.11 mol) in dry N,N-dimethylformamide (200 ml) was treated with sodium thiomethoxide (10 g, 0.14 mol) and the resulting mixture was heated under an atmosphere of nitrogen at 100° C. for 90 minutes. The mixture was stirred at room temperature for 72 hours and then reheated at 100° C. for a further 2 hours. The reaction mixture was cooled and diluted with water (1000 ml). A suspension was formed which was extracted twice with diethyl ether (500 ml). The combined organic layers were washed sequentially with water and brine, dried over anhydrous magnesium sulphate, filtered and evaporated under reduced pressure. The residue was azeotroped sequentially with diethyl ether and pentane to afford the title compound as a foam (48.9 g).

1. waitreheated at 100° C. for a further 2 hours
2. temperatureThe reaction mixture was cooled
3. customA suspension was formed which
4. extractionwas extracted twice with diethyl ether (500 ml)
5. washThe combined organic layers were washed sequentially with water and brine
6. dry with materialdried over anhydrous magnesium sulphate
7. filtrationfiltered
8. customevaporated under reduced pressure
9. customThe residue was azeotroped sequentially with diethyl ether and pentane