PDF《Supporting Information》

Supplementary Material (ESI) for Green Chemistry This journal is (c) The Royal Society of Chemistry

2010 S1 Clean chemical synthesis of 2-amino-chromenes in water catalyzed by nanostructured diphosphate Na2CaP2O7 Abderrahim Solhy,*a Abdelhakim Elmakssoudi,b Rachid Tahir,b Mohammed Karkouri,b Mohamed Larzek,b Mosto Bousmina,ac Mohamed Zahouily*ab a Institute of Nanomaterials &

Nanotechnology (INANOTECH), MAScIR Foundation (Moroccan Advanced Science, Innovation and Research), ENSET, Av.

De l'

Armée Royale, Madinat El Irfane

10100 - Rabat, Morocco. b Laboratoire de Catalyse, Chimiométrie et Environnement, URAC 24, Faculté des Sciences et Techniques, Université Hassan II, Mohammedia B. P. 146, 20650, Morocco. c Hassan II academy of Science and Technology, Rabat, Morocco. Email addresses: [email protected], [email protected] Supporting Information 1) General All commercial reagents were purchased from Aldrich Chemical Company. X-ray diffraction (XRD) patterns of the catalyst were obtained at room temperature on a Bruker AXS D-8 diffractometer using Cu-Kα radiation in Bragg-Brentano geometry (θ-2θ). Fourier transform infrared (FT-IR) spectra of samples in KBr pellets were measured on a Bruker Vector

22 spectrometer. SEM micrographs were recorded on a Hitachi S-4500 apparatus. The specific surface areas were determined from the nitrogen adsorption/desorption isotherms (at -196 C) measured with a Micromeritics ASAP

2010 automatic analyzer, using the BET equation at p/p0 = 0.98. The TEM micrographs were performed on a FEI microscope at

120 kV. NMR spectra were recorded on a Bruker ARX

300 spectrometer. Mass spectra were carried out on Polaris Q apparatus (Thermo-Electron), and the fragmentations were obtained by electronic impact (EI) at

70 eV. The data are given as mass-to-charge ratio (m/z), and nominal masses were used for the calculation of molecular weights of the prepared products. Melting points were determined using a Stuart SN5228 apparatus. Supplementary Material (ESI) for Green Chemistry This journal is (c) The Royal Society of Chemistry

2010 S2 2) Preparation and characterization of the catalyst The synthesis of the Na2CaP2O7 was carried out by the dry technique. The diphosphate Na2CaP2O7 was prepared is a white powder obtained starting from Na2CO3, CaCO3 and NH4H2PO4 in high purity grade and in 1:1:2 proportions, respectively. These materials were mixed together in an agate mortar and heated in porcelain crucible progressively to

873 K. However, it is necessary to make sure of the perfect homogeneity of the finished product and the total reaction of all the components. It requires, also, of many intermediate crushings after each heat treatment. The size of the finished product does not depend only on the quality of the starting products but also of the precision of the weighings and a good crushing. NH4H2PO4 + Na2CO3 + CaCO3 1) Grinding 2) Gradient heating *

383 K *

433 K 3) Grinding 4) Gradient heating *

473 K *

523 K *

623 K *

823 K 5) Grinding 6) Heating at

873 K 7) Grinding H20 NH3 CO2 Na2CaP2O7 Fig. S1 Preparation of Na2CaP2O7 Supplementary Material (ESI) for Green Chemistry This journal is (c) The Royal Society of Chemistry

2010 S3 Fig. S2 FT-IR spectrum of Na2CaP2O7 Table S1 Attribution of the observed bands of Na2CaP2O7 analyzed by FTIR spectroscopy Supplementary Material (ESI) for Green Chemistry This journal is (c) The Royal Society of Chemistry

2010 S4 Fig. S3 XRD patterns of Na2CaP2O7 3) Product characterizations (Note that copies of all NMR (1 H and