Ammonia → 6-Aminohexanenitrile
Reaction equation
[CH:1]([CH2:3][CH2:4][CH2:5][CH2:6][C:7]#[N:8])=O.[NH3:9]>[H][H]>[NH2:9][CH2:1][CH2:3][CH2:4][CH2:5][CH2:6][C:7]#[N:8].[NH2:9][CH2:1][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][NH2:8]Participants
Reactant 2
Product 2
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 80 °C
Procedure
In an autoclave having a capacity of 300 ml and equipped with a sampling sluice (material HC 4) there were placed 11 g of 5-formylvaleronitrile and 3 g of Ru (3%) on Al2O3 (4 mm extrudates) under protective gas (argon). The autoclave was then sealed and 150 ml of NH3 were forced in. Thorough mixing was effected using a magnetic stirrer. After heating to 80° C. (autogenous pressure: ca. 39 bar) the mixture was kept at 80° C. for a further 2 hours and then the overall pressure was raised, with hydrogen, to 70 bar. The pressure of 70 bar was maintained by constantly forcing in more hydrogen. After 25 hours, the autoclave was depressurized and the hydrogenation effluent analyzed by gas chromatography. The products formed comprised 73% of 6-aminocapronitrile and 12% of hexamethylene diamine. The conversion was 100%.
Workup
- customequipped with a sampling sluice (material HC 4) there
- customThe autoclave was then sealed
- additionThorough mixing
- temperatureThe pressure of 70 bar was maintained
- waitAfter 25 hours
Sources & evidence
- ORD record
- ord-63d24e8db18247ac85c4af57ca8484bc
- Source dataset
- uspto-grants-2000_09
- Patent number
- US06121481
Reaction notes
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