反应详情

Stir a mixture of 3-(4-pyridinylamino)-1H-indole-2-carboxylic acid (2.0 g, 8.0 mmol), chloromethyl diethylcarbamate (1.7 g, 10.4 mmol) and K2CO3 in DMF (50 mL) at ambient temperature overnight. Add EtOAc (400 mL), to the reaction mixture, wash the organic layer with brine solution (400 mL) and concentrate to an oil. Purify by flash chromatography over silica gel (40 g) eluting with EtOAc and then 10% MeOH/EtOAc. Collect like fractions and concentrate under vacuum to yield an oil. Crystallize from heptane-ether to obtain 1.1 g (36%) of the title compound as a white powder: MS 383(M+H).

1. washAdd EtOAc (400 mL), to the reaction mixture, wash the organic layer with brine solution (400 mL)
2. concentrationconcentrate to an oil
3. customPurify by flash chromatography over silica gel (40 g)
4. washeluting with EtOAc
5. customCollect like fractions
6. concentrationconcentrate under vacuum
7. customto yield an oil
8. customCrystallize from heptane-ether