Please do not adjust margins
Catalysis Science & Technology
Page 11 of 13
Journal Name
Synthesis of Fe3O4 nanoparticles:
DOI: 10.1039/C5CY00821B
ARTICLE
Notes and references
Magnetite (Fe3O4) nanoparticles were prepared according to
the reported method in the literature.13,14 Typically,
FeCl3.6(H2O) (11.0 g) and FeCl2.4H2O (4.0 g) were dissolved in
250 mL deionized water under argon with vigorous stirring
using mechanical stirrer. Then, aqueous ammonia (25%, 40
mL) was added dropwise under argon atmosphere and mixture
was stirred at 80 °C for 4 h. A black precipitate (Fe3O4) were
collected by external magnet and washed three times with
deionized water and ethanol and dried under vacuum.
1
(a) A. Suzuki, J. Organomet. Chem. 1999, 576, 147; (b)
M. Blangetti, H. Rosso, C. Prandi, A. Deagostino and P.
Venturello, Molecules 2013, 18, 1188. (c) F. Alonso, I. P.
Beletskaya and M. Yus, Tetrahedron 2008, 64, 3047; (d)
V. Polshettiwar, A. Decottignies, C. Len and A. Fihri,
ChemSusChem. 2010, 3, 502; (e) D. A. Alonso and C.
Najera, Chem. Soc. Rev. 2010, 39, 2891; (f) R. Rossi, F.
Bellina and M. Lessi, Adv. Synth. Catal. 2012, 354, 1181.
(g) G. A. Molander, S. R. Wisniewski and E. Etemadi-
Davan, J. Org. Chem. 2014, 79, 11199.
2
3
(a) R. F. Heck and J. P. Nolley, J. Org. Chem. 1972, 37,
Synthesis of silica-coated Fe3O4 nanoparticles
2320; (b) I. P. Beletskaya and A. Cheprakov, Chem. Rev.
2000, 100, 3009; (c) K. C. Nicolau, P. G. Bulger and D.
Sarlah, Angew. Chem., Int. Ed. 2005, 44, 4442; (d) F. I.
Alonso, I. P. Beletskaya and M. Yus, Tetrahedron 2005,
61, 11771; (e) A. Kumar, K. R. Gyandshwar, and A, K
To the 30 min sonicated Fe3O4 nanoparticles (1 g) in ethanol
(200 mL), were added tetraethyl orthosilicate (2 mL) and 6 mL
aqueous ammonia (6 mL) and mixture was stirred for 24 h at
room temperature. Produced SiO2@Fe3O4 nanoparticles were
separated by an external magnet and washed with H2O (3×10
mL) and EtOH (3×10 mL) and dried under vacuum.
Singh, RSC Adv., 2012,
Wong, Curr. Org. Synth. 2010,
(a) R. Chinchilla and C. Nájera, Chem. Rev. 2007, 107
2
, 12552; (f) H. Lin and P K.
7
, 599.
,
874; (b) R. Chinchilla and C. Nájera, Chem. Soc. Rev.
2011, 40, 5084; (c) R. Chinchilla and C. Nájera, Chem.
Rev. 2014, 114, 1783; (d) M. Karak, L. C. A. Barbosa
Synthesis of epoxy-functionalized magnetic nanoparticles (2)
and G. C. Hargaden, RSC Adv. 2014,
J. P. Christopher, W. Hau-to, F. C. Ferreira and A. G.
Livingston, Org. Process Res. Dev., 2008, 12, 589
S. Navalón, M. Álvaro and H. García, ChemCatChem.
2013, , 3460.
4, 53442.
Silica-coated Fe3O4 nanoparticles (1 g) were sonicated in 40 mL
dry toluene and 3-glycidoxypropyltrimethoxysilane (4 mmol,
0.9 mL) was added. The resulting mixture was refluxed for 24 h
under argon atmosphere. Then, the reaction mixture was
4
5
6
7
.
5
V. Polshettiwar and A. Molnár, Tetrahedron 2007, 63
6949.
,
subjected to magnetic separation, and obtained product (2)
was washed sequentially with H2O (3×10 mL) and EtOH (3×10
mL) and finally dried under vacuum.
(a) H. Veisi, A. A. Manesh, N. Eivazi and A. R. Faraji, RSC
Adv. 2015, , 20098; (b) L. Duan, R. Fu, Z. Xiao, Q. Zhao,
J.Q. Wang, S. Chen and Y. Wan, ACS Catal. 2015, , 575;
5
5
(c) H. Veisi, D. Kordestani, S. Hemmati, A. R. Faraji, H.
Veisi, Tetrahedron Lett. 2014, 55, 5311; (d) Z. Dong, K.
Synthesis of Im-Phos-SiO2@Fe3O4 (2)
The prepared epoxy-functionalized magnetic nanoparticles
2
Liang, C. Dong, X. Li, X. Lea and J. Ma, RSC Adv. 2015,
20987; (e) B. Karimi, H. Behzadnia and H. Vali,
ChemCatChem. 2014, , 745; (f) R. Ali Molla, M. A.
Iqubal, K. Ghosh, A. Singha Roy, Kamaluddin and Sk. M.
Islam, RSC Adv. 2014, , 48177; (g) P. Puthiaraj and K.
5,
(1 g) were sonicated in CH2Cl2 for 30 min. 1-Methyl imidazole
(4 mmol, 0.33 g) and chlorodiphenylphosphine (4 mmol, 0.88
g) were added under argon protection and reaction was stirred
6
4
°
at 50 C for 24 h. Then, produced phosphinite-imidazolium
Pitchumani, Green Chem. 2014, 16, 4223; (h) H. Veisi,
M. Hamelian, S. Hemmati, J. Mol. Catal. A: Chem. 2014,
395, 25; (i) H. Veisi, A. Amini Manesh, N. Eivazi, A. R.
functionalized magnetite was separated by external magnet
and washed three times with deionized water (2×10 mL) and
EtOH (3×10 mL) and dried under vacuum.
Faraji, RSC Adv., 2015, 5, 20098.
8
9
(a) F. Bellina and C Chiappe, Molecules 2010, 15, 2211;
(b) S.B. Park, H. Alper, Chem. Commun. 2004, 1306, (c)
N. Iranpoor, H. Firouzabadi and Y. Ahmadi, Eur. J, Org.
Chem. 2012, 305; (d) P. Nehra, B. Khungar, K.
Pericherla, S. C. Sivasubramaniana and A. Kumar,
Green Chem. 2014, 16, 4266.
Synthesis of magnetite supported palladium nanoparticle catalyst
(3)
The prepared Fe3O4@SiO2-Im-Phos (2) (1 g) was sonicated in
15 mL H2O. In another batch, PdCl2 (0.45 mmol, 0.08 g) were
°
sonicated in H2O (10 mL) at 80 C until dissolving PdCl2 salt.
(a) H. Firouzabadi, N. Iranpoor, M. Gholinejad, S. Akbari
and N. Jeddi, RSC Adv. 2014, 4, 17060; (b) F. Parra da
Then, the aqueous solution of PdCl2 was added to Fe3O4@SiO2-
Silva and L. Marcia Rossi, Tetrahedron 2014, 70, 3314;
(b) J. Kim, J. E. Lee, J. Lee, Y. Jang, S.-W. Kim, K. An, J. H.
Yu and T. Hyeon, Angew. Chem. Int. Ed. 2006, 45, 4789;
(c) S. Verma, D. Verma, A. K. Sinha and S. L. Jain, Appl.
Catal. A: General 2015, 489, 17; (d) Z. Yinghuai, S. C.
Peng, A. Emi, S. Zh. Monalisa and R. A. Kemp, Adv.
Synth. Catal. 2007, 349, 1917; (e) C. G. Tan and R. N.
Grass, Chem. Commun. 2008, 4297; (f) S. Shylesh, L.
Im-Phos (2
) and the mixture was stirred at 60 °C for 24 h. Next,
the mixture was subjected to magnetic separation and the
solid was washed with H2O (3×10 mL) and EtOH (3×10 mL) and
dried under vacuum.
Wang and W. R. Thiel, Adv. Synth. Catal. 2010, 352
,
Acknowledgements
425; (g) D. Yuan, Q. Zhang and J. Dou, Catal. Commun.
2010, 11, 606; (h) R. Cano, D. J. Ramón and M. Yus,
Tetrahedron 2011, 67, 5432; (i) R. Cano, M. Yus and D.
J. Ramón, Tetrahedron 2011, 67, 8079; (j) P. Li, L.
Wang, L. Zhang, and G. W. Wang, Adv. Synth. Catal.
The authors are grateful to Institute for Advanced Studies in
Basic Sciences (IASBS) Research Council and Iran National
Science Foundation (INSF-Grant number of 92027195) for the
support of this work.
This journal is © The Royal Society of Chemistry 20xx
J. Name., 2013, 00, 1-3 | 11
Please do not adjust margins