反应详情

Under a nitrogen atmosphere 910 mg (14.5 mmol) sodium cyanoborohydride was added batchwise to 1.0 g (4.83 mmol) methyl (5-fluoro-1H-indol-3-yl)-acetate in 12.5 g acetic acid while cooling slightly. After 2 h stirring at RT another 910 mg (14.5 mmol) sodium cyanoborohydride was added batchwise while cooling slightly. After 3 h stirring at RT the solvent was evaporated down using the rotary evaporator. The residue was taken up in 4M hydrochloric acid and stirred for 30 min. Then the reaction solution was made alkaline with solid potassium carbonate and extracted with dichloromethane (3×). The combined organic phases were dried on sodium sulphate, filtered and evaporated down using the rotary evaporator. The product thus obtained was reacted directly.

1. temperaturewhile cooling slightly
2. additionwas added batchwise
3. temperaturewhile cooling slightly
4. customwas evaporated down
5. customthe rotary evaporator
6. stirringstirred for 30 min
7. extractionextracted with dichloromethane (3×)
8. customThe combined organic phases were dried on sodium sulphate
9. filtrationfiltered
10. customevaporated down
11. customthe rotary evaporator
12. customThe product thus obtained
13. customwas reacted directly