反应详情

温度

70 °C

Under an argon atmosphere 1.6 g (8.7 mmol) 5,6-difluoro-3-methyl-1,3-dihydro-indol-2-one were placed in 50 mL THF. 18 mL (18 mmol) 1 M borane in THF were slowly added dropwise. The reaction mixture was stirred for 2 h at 70° C. After cooling to RT 10 mL methanol and 30 mL semiconc. HCl were successively added dropwise and then the mixture was refluxed for 1 h. After cooling to RT it was extracted with EtOAc. The aqueous phase was made alkaline with 4M NaOH solution and extracted with DCM. The organic phase was dried, filtered and evaporated down.

1. temperaturethe mixture was refluxed for 1 h
2. temperatureAfter cooling to RT it
3. extractionwas extracted with EtOAc
4. extractionextracted with DCM
5. customThe organic phase was dried
6. filtrationfiltered
7. customevaporated down