反应详情

温度

-75 °C

To a stirring solution of 2,3-dihydro-1H-indole-5-sulfonic acid thiazol-2-ylamide (2.35 g, 8.36 mmol) in DMF (10 mL), at −75° C., was added triethylamine (1.16 mL, 8.36 mmol) followed by chloroacetyl chloride (1.88 g, 16.7 mmol). The mixture was stirred at −75° C. for 1 h. The reaction showed product formation by LC/MS (10-99% CH3CN). After quenching with MeOH and allowing the mixture to warm to room temperature, the solvents were removed in vacuo. The mixture was purified via column chromatography (2% MeOH in CH2Cl2) to obtain the desired amide (1.95 g, 5.9 mmol, 70% yield). LC/MS (10-99% CH3CN), M/Z: M+1 obs=359.3; tR=2.46 min.

1. customAfter quenching with MeOH
2. temperatureto warm to room temperature
3. customthe solvents were removed in vacuo
4. customThe mixture was purified via column chromatography (2% MeOH in CH2Cl2)