反应详情

温度

45 °C

Raney nickel (6.7 g) was added to a solution of 5-cyanoindole (Aldrich, 10.0 g) and sodium hypophosphite (20.0 g) in a mixture of water (73 ml), glac. acetic acid (73 ml) and pyridine (145 ml) at 45° C. The resulting mixture was stirred at 45° C. for 2 hours, then cooled and filtered through Hyflo. The filtrate was diluted with water and extracted with ethyl acetate. The combined extracts were washed with water, 10% aqu. citric acid. IN aqu. HCl, water and brine, dried and evaporated in vacuo to give the desired product as a buff solid which was recrystallised from chloroform (7.5 g).

1. customat 45° C
2. temperaturecooled
3. filtrationfiltered through Hyflo
4. additionThe filtrate was diluted with water
5. extractionextracted with ethyl acetate
6. washThe combined extracts were washed with water, 10% aqu
7. dry with materialHCl, water and brine, dried
8. customevaporated in vacuo