DL-Pipecolinic acid synthesis

12synthesis methods

Product Name:DL-Pipecolinic acid
CAS Number:4043-87-2
Molecular formula:C6H11NO2
Molecular Weight:129.16

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Yield:4043-87-2 43%

Reaction Conditions:

with hydrogen;5%-palladium/activated carbon in water at 200; under 5171.62 Torr; for 8 h;Product distribution / selectivity;

Steps:

1

Hydrodenitrogenation of L-Lysine in Water. L-Lysine hydrochloride (1.83 g, 10 mmol), water (100 mL) and Raney Ni (0.58 g, 10 mmol) are added to the reaction chamber of a Parr high-pressure reactor and the vessel is assembled. The reaction chamber is flushed for 10 min with Ar and then pressurized with H₂ to 100 psi (689.48 kPa). The reaction chamber's outlet valve is then opened to the atmosphere. This process is repeated two additional times. After repressurizing the reaction vessel with 100 psi of H₂, the temperature of the stirred reaction vessel is increased to 200⁰C, which results in a reaction pressure of 300 psi. The reaction is held at 200⁰C for 8 h. Upon cooling to rt (room temperature), the pressurized reaction vessel's H₂ is vented in a fume hood. After filtration, the reaction solution is concentrated.

References:

WO2008/103366,2008,A2 Location in patent:Page/Page column 17, 19