反应详情

温度

60 °C

To the solution of benzyl 4-methyl-3-(2-(5-tosyl-5H-pyrrolo[2,3-b]pyrazin-2-ylamino)acetyl)piperidine-1-carboxylate (1.2 g, 2.2 mmol) in 1,4-dioxane (15 mL) was added Lawesson's reagent (0.44 g, 1.1 mmol) and the mixture was heated at about 60° C. for about 90 min. The solvent was removed under reduced pressure and the residue was purified by silica gel chromatography eluting with a gradient of 0-1.5% MeOH/DCM to yield benzyl 4-methyl-3-(3-tosyl-3H-imidazo[1,2-a]pyrrolo[2,3-e]pyrazin-8-yl)piperidine-1-carboxylate (0.93 g, 78%) as a yellow amorphous solid: LC/MS (Table 2, Method a) Rt=2.49 min; MS m/z: 544 (M+H)+.

1. customThe solvent was removed under reduced pressure
2. customthe residue was purified by silica gel chromatography
3. washeluting with a gradient of 0-1.5% MeOH/DCM