反应详情

温度

60 °C

To a well stirred solution of conc. H2SO4 (28.5 mL) and methyl isoquinoline-4-carboxylate (5.0 g, 26.7 mmol) at 0° C. was added, NCS (35.7 g, 267 mmol) slowly and the reaction mixture was allowed to come to RT and then heated to 60° C. overnight. After completion (TLC), it was quenched with ice, neutralized (NaHCO3) and extracted with EtOAc (100 mL×3). The organic phase was separated, dried (Na2SO4) and concentrated to give dark brown oil (4.6 g) as crude product that was purified by flash column chromatography (15% EtOAc in Hexanes) to furnish the desired compound (3.8 g, 64%) as pale yellow oil.

1. customto come to RT
2. customAfter completion (TLC), it was quenched with ice
3. extractionextracted with EtOAc (100 mL×3)
4. customThe organic phase was separated
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated