反应详情

温度

110 °C

Into an inertised reactor with a capacity of 150 ml provided with a turbine agitator were successively introduced 41.9 g benzaldehyde (395.3 mmol), 20.1 g CH3OH, 0.08 g 5% palladium/carbon (Degussa; E10 R/W 50% H2O w/w) and 3.8g NH3 (223.5 mmol). The reactor was then pressurized to 70 bar with hydrogen. Next, the temperature was raised to 110° C. and the pressure in the reactor increased to 85 bar with hydrogen. After approximately 15 minutes no further hydrogen was absorbed. The reactor contents were cooled to room temperature and the reactor was then depressurized and flushed with N2. After the catalyst had been filtered off, the reaction mixture was found to be a 2-phase system. This 2-phase system was homogenized after the addition of the CH3OH which was used for flushing of the autoclave. The homogenous reaction mixture obtained in this way was analyzed by means of gas chromatography. All the benzaldehyde had been completely converted. The selectivity to dibenzylamine was 95.1%. In addition, small amounts of benzylalcohol (sel. approx. 1.8%) and tribenzylamine were formed.

1. customInto an inertised reactor with a capacity of 150 ml provided with a turbine agitator
2. customAfter approximately 15 minutes no further hydrogen was absorbed
3. temperatureThe reactor contents were cooled to room temperature
4. customflushed with N2
5. filtrationAfter the catalyst had been filtered off
6. additionafter the addition of the CH3OH which
7. customfor flushing of the autoclave
8. customThe homogenous reaction mixture obtained in this way