反应详情

温度

0 °C

To a stirred suspension of 60% NaH dispersion in mineral oil (78.8 mg, 2.0 mmol) in DMF (2.5 mL) cooled to 0° C. is added a solution of diethyl 1H-indole-2,6-dicarboxylate (Intermediate A, 561 mg, 2.1 mmol) in DMF (3 mL). The mixture is stirred for 20 min and a solution of tert-butyl 6-methyl-1,2,3-oxathiazinane-3-carboxylate 2,2-dioxide (450 mg, 1.8 mmol) in DMF (2.5 mL) is added. The reaction mixture is stirred for 30 min at 0° C. and it is warmed to room temperature and stirred for 48 h. Saturated NH4Cl solution is added and the reaction mixture is extracted with EtOAc. The organic layer is separated, washed with water, then brine, dried (MgSO4) and concentrated to afford the title compound (1.04 g, 50% pure) as an oil.

1. stirringThe reaction mixture is stirred for 30 min at 0° C.
2. temperatureit is warmed to room temperature
3. stirringstirred for 48 h
4. extractionthe reaction mixture is extracted with EtOAc
5. customThe organic layer is separated
6. washwashed with water
7. dry with materialbrine, dried (MgSO4)
8. concentrationconcentrated