反应详情

温度

200 °C

N-((7-Amino-8-benzyl-5,6,7,8-tetrahydronaphthalen-2-yl)methyl)-1-cyclopropylmethanesulfonamide (0.083 g, 0.216 mmol) and 3-oxetanone (0.031 g, 0.432 mmol) were sealed in a vial and heated at 200° C. for 2 minutes. Trimethylsilyl cyanide (0.58 mL, 0.432 mmol) was added, the vial was resealed and the mixture was heated again at 200° C. for 2 minutes. The mixture was diluted with ethyl acetate (40 mL) and washed with 1N NaOH (1×20 mL) and brine (1×20 mL). The organic extract was collected, dried on MgSO4 and evaporated under reduced pressure to give a brown oil. The residue was purified by flash-chromatography on silica gel (100% heptane then up to 60% ethyl acetate in n-heptane). (24.9 mg, 0.048 mmol, 22.3%).

1. temperaturethe mixture was heated again at 200° C. for 2 minutes
2. washwashed with 1N NaOH (1×20 mL) and brine (1×20 mL)
3. extractionThe organic extract
4. customwas collected
5. customdried on MgSO4
6. customevaporated under reduced pressure
7. customto give a brown oil
8. customThe residue was purified by flash-chromatography on silica gel (100% heptane