反应详情

Compound 131 (4.68 g, 11.2 mmol) was dissolved in THF (100 ml), NaHCO3 (s) (appr. 5 ml) was added followed by phosgene-solution (20% in toluene, 11.6 ml, 22.5 mmol). The reaction mixture was stirred vigorously for 1 h and then filtrated, evaporated and redissolved in DCM (100 ml). NaHCO3 (s) (appr. 5 ml) was added followed by hept-6-enyl-(4-methoxy-benzyl)-amin (3.92 g, 16.8 mmol). The reaction mixture was stirred at room temperature overnight, filtrated and evaporated on silica. The crude product was purified by column chromatography on silica (EtOAc/n-Heptane 25/75) to give the title compound (6.9 g, 91%).

1. filtrationfiltrated
2. customevaporated
3. dissolutionredissolved in DCM (100 ml)
4. additionNaHCO3 (s) (appr. 5 ml) was added
5. stirringThe reaction mixture was stirred at room temperature overnight
6. filtrationfiltrated
7. customevaporated on silica
8. customThe crude product was purified by column chromatography on silica (EtOAc/n-Heptane 25/75)