反应详情

Under a nitrogen atmosphere 41 mL (41 mmol) of a 1M borane in THF solution was added dropwise to 2.2 g (14 mmol) 3-ethylidene-1,3-dihydro-indol-2-one in 50 mL THF. The reaction mixture was refluxed for 3 h and then at 0° C. mixed with 10 mL methanol followed by 15 mL semi-concentrated hydrochloric acid solution. The reaction mixture was refluxed for 3 h with stirring, cooled and washed twice with ethyl acetate. The aqueous phase was made alkaline with aqueous 4M sodium hydroxide solution and extracted three times with ethyl acetate. The organic phases were combined, dried on sodium sulphate and evaporated down.

1. temperatureThe reaction mixture was refluxed for 3 h
2. temperatureThe reaction mixture was refluxed for 3 h
3. temperaturecooled
4. washwashed twice with ethyl acetate
5. extractionextracted three times with ethyl acetate
6. customdried on sodium sulphate
7. customevaporated down