The hydrogenation was performed on a 4712 model Parr
reactor. In a Schlenk tube under nitrogen atmosphere, corresponding
b-enamino ester (100 mg, 0.037 mmol) was added to a
solution of Co2(CO)8 (1 mol%), (R)-BINAP (2mol%) and PPh3 (2 mol
%) in THF (10 mL), the reaction mixture was stirred for 10 min.
Then, the solution was transferred to a 45 mL steel Parr vessel
previously purged with vacuum-nitrogen. The reaction vessel was
pressurized at 450 psi with a H2/CO mixture in a 1/3 ratio. The
reactor was placed in a preheated oil bath at 120 with magnetic
stirring for 36 h. At the end of the reaction time, the reactor was
cooled and the gases were liberated. The solution was concentrated
under reduced pressure and resulting product was purified
by chromatography column using hexane and ethyl acetate as
eluents.
The hydrogenation was performed on a 4712 model Parrreactor. In a Schlenk tube under nitrogen atmosphere, correspondingb-enamino ester (100 mg, 0.037 mmol) was added to asolution of Co2(CO)8 (1 mol%), (R)-BINAP (2mol%) and PPh3 (2 mol%) in THF (10 mL), the reaction mixture was stirred for 10 min.Then, the solution was transferred to a 45 mL steel Parr vesselpreviously purged with vacuum-nitrogen. The reaction vessel waspressurized at 450 psi with a H2/CO mixture in a 1/3 ratio. Thereactor was placed in a preheated oil bath at 120 with magneticstirring for 36 h. At the end of the reaction time, the reactor wascooled and the gases were liberated. The solution was concentratedunder reduced pressure and resulting product was purifiedby chromatography column using hexane and ethyl acetate aseluents.
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