反应详情

温度

60 °C

Add 2,2-dimethyl-2H-chromene-6-carbonitrile (1.5 g, 8.1 mmol) and ethanol wet Raney® activated nickel (0.4 g) to a Parr pressure vessel. Immediately add 7N ammonia in methanol (170 mL) and seal the vessel. Purge the reaction vessel with nitrogen, pressurize the reaction mixture with hydrogen (3400 KPa), seal the vessel, agitate the reaction and heat to 60° C. for 20 h. Turn off the heat and allow the reaction mixture to cool to ambient temperature. Vent the excess hydrogen from the vessel and purge the vessel with nitrogen. Filter the reaction mixture to remove the Raney® nickel. Purify by chromatography on silica gel eluting with DCM/2M ammonia in methanol (9:1) to obtain the title compound (1.5 g, 97%). MS (ES+) m/z: 175 M+H−NH3)+.

1. customPurge the reaction vessel with nitrogen
2. customseal the vessel
3. customthe reaction
4. temperatureheat
5. temperatureto cool to ambient temperature
6. customVent the excess hydrogen from the vessel and purge the vessel with nitrogen
7. filtrationFilter the reaction mixture
8. customto remove the Raney® nickel
9. customPurify by chromatography on silica gel eluting with DCM/2M ammonia in methanol (9:1)