反应详情

温度

70 °C

Under an argon atmosphere 0.30 g (1.8 mmol) 5,6-difluoroxindole were dissolved in 10 mL THF and 3.0 mL of a 1 molar borane solution in THF were added dropwise. Then the reaction mixture was heated to 70° C. for 2 h and then cooled. After mixing with 3 mL MeOH another 5 mL of a 4N aqueous hydrochloric acid solution were added and the mixture was refluxed for 1 h. The organic phase was evaporated down, the aqueous phase was washed with DCM and then made alkaline with a 4N aqueous sodium hydroxide solution and extracted several times with EtOAc. The combined organic phases were dried on sodium sulphate, filtered and evaporated down.

1. temperaturecooled
2. additionwere added
3. temperaturethe mixture was refluxed for 1 h
4. customThe organic phase was evaporated down
5. washthe aqueous phase was washed with DCM
6. extractionextracted several times with EtOAc
7. customThe combined organic phases were dried on sodium sulphate
8. filtrationfiltered
9. customevaporated down