反应详情

温度

70 °C

A solution of tert-butyl 4-[(6-bromo-1-oxo-1,2-dihydroisoquinolin-4-yl)methyl]piperazine-1-carboxylate (Example 27b, 0.171 g) dissolved in DMF (5 mL) was treated with cesium carbonate (0.264 g) and [1-({[tert-butyl(dimethyl)silyl]oxy}methyl)cyclobutyl]methyl methanesulfonate [Archiv der Pharmazie (Weinheim, Germany), 2005, 338 (11), 522-7] (0.187 g) under nitrogen. The resulting mixture was stirred at 70° C. for 7 h. The reaction was diluted with water (300 mL), and extracted with diethyl ether (300 mL×3). The organic was dried (MgSO4), filtered and evaporated to afford crude product. The crude product was purified (SiO2 chromatography, elution with 6-12% ethyl acetate/isohexane) to afford the subtitle compound (0.153 g).

1. extractionextracted with diethyl ether (300 mL×3)
2. dry with materialThe organic was dried (MgSO4)
3. filtrationfiltered
4. customevaporated
5. customto afford crude product
6. customThe crude product was purified
7. wash(SiO2 chromatography, elution with 6-12% ethyl acetate/isohexane)