反应详情

Under an argon atmosphere 0.30 g (1.8 mmol) 5,6-difluoro-1,3-dihydro-indol-2-one were dissolved in 10 mL THF and 3.0 mL of a 1 M borane in THF solution were added dropwise. Then the reaction mixture was heated for 2 h to 70° C. and then cooled. After the addition of 3 mL MeOH a further 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. temperatureThen the reaction mixture was heated for 2 h to 70° C.
2. temperaturecooled
3. additionwere added
4. temperaturethe mixture was refluxed for 1 h
5. customThe organic phase was evaporated down
6. washthe aqueous phase was washed with DCM
7. extractionextracted several times with EtOAc
8. customThe combined organic phases were dried on sodium sulphate
9. filtrationfiltered
10. customevaporated down