반응 #474458

반응 방정식

5-bromo-3-(2,6-dimethyl-1,1-dioxidotetrahydro-2H-thiopyran-4-yl)-1H-indole-7-carboxylic acid

EDC

HOBt

Ammonia

1,4-dioxane

→

title compound

수율 80.4%

5-Bromo-3-(2,6-dimethyl-1,1-dioxidotetrahydro-2H-thiopyran-4-yl)-1H-indole-7-carboxamide

수율 80.4%

용매

water

DMF

반응 조건

후처리

1. 1
   추출extracted with Ethyl acetate
2. 2
   세척The combined organics were washed with 2× water, 2×1N NaOH, brine
3. 3
   건조then dried with magnesium sulfate

실험 절차

5-bromo-3-(2,6-dimethyl-1,1-dioxidotetrahydro-2H-thiopyran-4-yl)-1H-indole-7-carboxylic acid (0.187 g, 0.467 mmol) was suspended in DMF (3 mL) with EDC (0.269 g, 1.40 mmol, 3 eq) and HOBt (0.072, 0.467 mmol) in a 10 mL microwave reaction vessel. 0.5M Ammonia in 1,4-dioxane (0.93 mL, 0.467 mmol) was added and heated on the microwave at 100° C. for 20 minutes. The reaction was diluted with water and extracted with Ethyl acetate. The combined organics were washed with 2× water, 2×1N NaOH, brine then dried with magnesium sulfate, to give 0.150 g (80%) of the title compound.

출처