ACS Catalysis
Research Article
charged into a 50 mL Hastelloy-C high-pressure Parr reactor.
The resulting mixture was vigorously stirred (800 rpm) under
an N2 atmosphere (5 atm) at the designed temperature for the
given reaction time. After completion of the reaction, the
reaction mixture was filtered and the catalyst was washed
thoroughly with ethanol. Then the filtrate was concentrated
and dried under reduced pressure using a rotary evaporator.
The crude product was purified by column chromatography
(silica gel (200−300 mesh); petroleum ether (60−90 °C)/
ethyl acetate mixture) to afford the product. All of the products
Additional data and explanations as described in the text
AUTHOR INFORMATION
■
Corresponding Author
ORCID
Notes
1
were identified by H NMR and 13C NMR, and the spectra
The authors declare no competing financial interest.
obtained were compared with the standard spectra. The
conversion and yields were determined with an Agilent
7820A gas chromatograph equipped with a HP-INNOWax
column (30 m × 0.32 mm × 0.25 μm) and a flame ionization
detector (FID).
ACKNOWLEDGMENTS
■
This work was supported by the NSF of China (21273044,
21473035, 91545108), the Science & Technology Commission
of Shanghai Municipality (16ZR1440400), and the Open
Project of State Key Laboratory of Chemical Engineering
(SKL-ChE-15C02).
4.2. Procedure for Large-Scale Condensation of 2,5-
Dimethylfuran with m-Methylaniline under Neat Con-
ditions. A mixture of 2,5-dimethylfuran (100 mmol), m-
methylaniline (100 mmol), and H-Y (2.6) (150 mg) were
charged into a 50 mL Hastelloy-C high-pressure Parr reactor.
The resulting mixture was vigorously stirred (800 rpm) under
an N2 atmosphere (5 atm) at 180 °C for 18 h. After completion
of the reaction, the reaction mixture was filtered and the
catalyst was washed thoroughly with ethanol. Then the filtrate
was concentrated and dried under reduced pressure using a
rotary evaporator. The crude product was purified by column
chromatography (silica gel (200−300 mesh); petroleum ether
(60−90 °C)/ethyl acetate mixture) to afford the product. All of
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ACS Catal. 2017, 7, 959−964