反应详情

温度

0 °C

To a 0° C. solution of 0.18 mmol 3-bromo-6-trityl-6,7-dihydro-5H-pyrrolo[3,4-b]pyridine in 0.5 ml chloroform and 0.5 ml methanol was added dropwise 1 ml trifluoroacetic acid. After 5 minutes stirring at 0° C. and 30 minutes at RT, the reaction mixture was concentrated. The residue was taken in water/ether and 1 ml 1N HCl was added. The aqueous phase was extracted with ether (2 times), then basified with 5N NaOH and extracted with dichloromethane (3 times). Combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo to yield the title compound as a light yellow solid. MS (m/e): 199.0 (M+, 100%)

1. concentrationthe reaction mixture was concentrated
2. addition1 ml 1N HCl was added
3. extractionThe aqueous phase was extracted with ether (2 times)
4. extractionextracted with dichloromethane (3 times)
5. dry with materialCombined organic phases were dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo