Avance DRX in pure deuterated DMSO-d6 and CDCl3 solvents with tetramethylsilane (TMS) as internal standards. Mass spectra recorded on a FINNIGAN-MAT 8430 mass spectrometer operating at 70eV. X-ray diffraction selleck (XRD, D8, Advance, Bruker, axs) and FT-IR spectroscopy (Shimadzu FT-IR 8300 spectrophotometer) were employed for characterization of the PNP-SBNPM sorbent. Melting points were determined in open capillary tubes in a Barnstead Electrothermal 9100 BZ circulating oil melting point apparatus. TLC accomplished the reaction monitoring on silica gel PolyGram SILG/UV254 plates. Column chromatography was carried out on columns of silica gel 60 (70�C230 mesh). Pd nanoparticles on silica-bonded N-propyl morpholine (PNP-SBNPM) were synthesized according to the literature [16] and illustrated in Figure 1.
Figure 1Preparation of PNP-SBNPM catalyst. (a) (3-chloropropyl) trimethoxysilane, toluene, reflux, 18h. (b) Morpholine, CHCl3, Et3N, 8h. (c) Pd(OAC)2, ethanol, r.t, 12h. (d) Washing with ethanol. (e) Washing with ether.2.3. Preparation of Immobilized Palladium Nanoparticles on Silica-Functionalized Morpholine2.3.1. Silica-Bonded N-Propyl Morpholine To a magnetically stirred mixture of 3-chloropropylsilica (5g) in dry CHCl3 (20mL), morpholine (0.157g, 1.8mmol) and some drops of triethyl amine were added and refluxed for 24h. Then, the mixture was filtered and washed with dichloromethane (3 �� 10mL) and ethanol (3 �� 10mL). After drying in oven, silica-bonded N-propyl morpholine (SBNPM) was obtained as white powder (5.15g).2.3.2.
Pd Nanoparticles on Silica-Bonded N-Propyl Morpholine (PNP-SBNPM) To a mixture of silica-bonded N-propyl morpholine (SBNPM) (1g) in ethanol (10mL), palladium acetate (0.15g, 0.67mmol) was added and stirred 24h at room temperature. Then, the mixture was filtered and washed with ethanol (3 �� 10mL). After drying in vacuum oven Pd nanoparticles loaded on silica bonded, N-propyl morpholine (PNP-SBNPM) was obtained as dark solid (1.1g) (Figure 1).2.4. Attachment of Palladium Nanoparticle to the Silica Gel Anacetrapib Functionalized with N-Propyl MorpholineThe palladium nanoparticles silica-bonded N-propyl morpholine (PNP-SBNPM) was produced via the reaction of silica-bonded N-propyl morpholine (SBNPM) with palladium acetate in ethanol [16�C22]. For preparation of SBNPM, 3-chloropropylsilica (3-CPS) treatment with morpholine and 3-CPS was produced by the reaction of activated silica with 3-chloropropyl trimethoxysilane (Figure 1). The proposed sorbent also was studied by Fourier FT-IR (Figure 2(a)) as a powerful functional group recognition. As it can be seen, appearance of new peaks around 470.6 (1cm?1), 470.6 (1cm?1), 802.3 (1cm?1), 968.2 (1cm?1), 1562.2 (1cm?1), 2337.6 (1cm?1), 3444.