反应详情

Boron trifluoride ethyl etherate (0.135 g, 0.12 mL, 0.001 mol) was added to a mixture of ethyl 5-chloro-6-fluoroindole-2-carboxylate (0.75 g, 0.0031 mol), N-(3,5-dimethylphenylthio)-succinimide (0.78 g, 0.0033 mol) and anhydrous dichloromethane (20 mL) under dry argon atmosphere. After stirring at room temperature for 2 hours was added boron trifluoride ethyl etherate (0.27 g, 0.24 mL, 0.002 mol) and then reaction was heated at 45° C. for 2 hours. After cooling reaction was diluted chloroform and brine while shaking. Organic layer was separated, washed with saturated solution of sodium hydrogen carbonate, then with brine and dried. The solvent was evaporated to give 1.2 g (100%) of satisfactory pure title compound, mp 170-173° C. (from ethanol).

1. customreaction
2. temperaturewas heated at 45° C. for 2 hours
3. temperatureAfter cooling
4. customreaction
5. stirringwhile shaking
6. customOrganic layer was separated
7. washwashed with saturated solution of sodium hydrogen carbonate
8. dry with materialwith brine and dried
9. customThe solvent was evaporated