To a stirred solution of acetanilide (2gm, 0.5moles) in dry acetonitrile (5ml) at 0-5⁰C, TiCl4 (2.8gm, 1.0moles) was added drop wise with stirring and the mixture was stirred at room temperature for 30 min. Then Sodium azide (0.93gm, 0.5 mol.) was added to it and the reaction mixture was heated at 80-90⁰C. After 2 hrs remaining amount of sodium azide (0.93gm, 0.5 mol.) was added to reaction mixture and heating was continued for 4-6 hrs. The reaction was monitored by TLC after 3hrs. Then the reaction mixture was cooled and poured over crushed ice and the product separated out was filtered, washed with water, dried and recrystallized from alcohol. 5-Methyl-1-phenyl-1H-tetrazole (1). White crystals; yield 87 %; mp. 103 ⁰C; 1H-NMR (CDCl3): δ 7.48 …show more content…
Light yellow crystals; yield 87 %; mp. 152 ⁰C; 1H-NMR (CDCl3): δ 8.48 (m, 1H), 8.40 (m, 1H); 8.11 (m, 1H), 7.80 (m, 1H); 2.49(s, 3H); FT-IR: 3080, 2997, 1614, 1583, 1527, 1496, 1435, 1354, 1298, 1109, 1080, 1030, 910, 842, 806, 752 …show more content…
Light yellow crystals; yield 87 %; mp. 118 ⁰C; 1H-NMR (CDCl3): δ 8.41 (m, 1H), 8.22 (m, 1H); 7.92 (m, 1H), 7.75 (m, 1H); 2.15(s, 3H); FT-IR: 3093, 2989, 1608, 1581, 1527, 1496, 1411, 1344, 1305, 1280, 1257, 1112, 1089, 1024, 987, 854, 750, 723 cm-1. 5-methyl-1-(4-fluorophenyl)-1H-tetrazole (2). White crystals; yield 87 %; mp. 82 ⁰C; 1H-NMR (CDCl3): δ 7.65 (dd, 2H), 7.39 (dd, 2H); 2.42(s, 3H); FT-IR (KBr): 3120, 2983, 1600, 1514, 1411, 1383, 1274, 1230, 1157, 1093, 1041, 989, 839, 690, 613 cm-1. 1-(4-bromophenyl)-5-methyl-1H-tetrazole (2). White crystals; yield 87 %; mp. 118 ⁰C; 1H-NMR (CDCl3): δ 7.75 (dd, 2H), 7.58 (dd, 2H); 2.45(s, 3H); FT-IR: 3084, 2983, 2879, 1516, 1492, 1408, 1273, 1118, 1101, 1076, 1039, 1008, 844, 821 cm-1. Conclusion. In conclusion, we have developed a novel protocol for high yielding method for the synthesis of 1,5-disubstituted tetrazoles from secondary amides using TiCl4 as a catalyst for first time. The use of TiCl4 enhances the reactivity of inexpensive sodium azide towards secondary amides. This methodology may be used efficiently for the synthesis of variety of 1,5-disubstituted tetrazoles. Acknowledgements. Authors are thankful to the Principal, S. M. D. Mohekar College, Kalamb and S. C. Shivaji College, Omerga for providing laboratory
Therefore, the hydrate is probably CuSO4•5H2O. However, the percentage of error, 7.224%, is not small enough, and the crystals turn out to have a yellowish green color instead of to be white. This can be eliminated by decreasing the amount of hydrate, avoid touching the hydrate with other substances during the reaction, and increasing the intensity of the flame and the time of
A spin vane was added and a water-jacked condenser was attached. Isopentyl nitrite (0.06ml, 0.045 mmol) was dissolved in 1,2-dimethoxyethane (0.50 ml) in a 3-ml conical vial and caped to prevent loss by evaporation. Running the reaction. The mixture in the 5-ml conical vial containing the tetraphenylcyclopentadienone and anthranilic acid was heated on an aluminum block to 140° C. Once the mixture started to boil the prepared mixture of isopentyl nitrite was added to the 5-ml conical vial through the top of the condenser using a pasture pipette.
It is located in the Actinide metals section and also the F-block. Chemical Properties: Reaction with air: - When plutonium is exposed to air it begins to oxidise, it forms a yellowish-brown outer coat and begins to tarnish. Soluble in: - Hydrochloric acid Insoluble in: - Nitric acid - Concentrated hydrogen sulfide
Lecturer Date Introduction Theoretical Background Procedure The procedure was segmented into two categories, the reaction set up and the crude product isolation. Reaction set up The magnetic stirrer was prepared through placing it in the fume cupboard. 1 mmol of L-Phenylalanine was placed and weighed in a 5 mL conical vial.
The TLC plates were visualized by spraying with vanillin- HCl reagent resulting in a UV sensitive band, which on heating, developed green color. The UV sensitive bands were purified using repetitive preparative TLC followed by crystallization. The identity of Ecdysterone was established by the following procedure: HPLC, with a Shimadzu LC-20, a Phenomenex C-18 reverse-phase Luna C18 which was used with a mobile phase of MeOH:Water (1:1) at 1.80 mL/min and the absorbance was monitored at 254 nm. Studies confirming the presence of a single peak of the isolated Ecdysterone, with a characteristic UV absorption at 246 nm were done using commercial standard Ecdysterone (Sigma) (Figure 2 A and B).
This drug treats breast, ovarian, pancreatic, lung, and bladder cancer. When cells are not working correctly in the body this causes a problem, the cells start to mutate and things start happening to the body, such as cancer. The chemical formula and structure for Gemzar. The chemical formula for Gemzar is C9H11F2N3O4. The chemical structure for Gemcitabine
TLC was used to identify the actual unknown product as well as other products/reactants present in the filtered solution. The procedure was conducted by placing a TLC plate in a developing chamber that is filled with a small amount of solvent. The solvent cannot be too polar because it will cause spotted compounds on the TLC plate to rise up too fast, while a very non-polar solvent will not allow the spots to move. The polarity of the spots also determines how far it moves on the plate; non-polar spots are higher than polar ones. After spots on the TLC form, the Rf values are calculated and used to analyze the similarity of the compounds.
This family of natural products possesses a unique 4,8-dioxabicyclo[3.2.1]octane core, and vary in their 1-alkyl and their 6-acyl side chains. “ ZARAGOZIC ACID A ”
5.2. POVIDONE78, 79: Nonproprietary Names: BP: Povidone, USP: Povidone Synonyms: E1201; Kollidon; Plasdone; poly[1-(2-oxo-1-pyrrolidinyl)ethylene]; polyvidone; polyvinylpyrrolidone; PVP; 1-vinyl-2-pyrrolidinone polymer. Chemical Name and CAS Registry Number: 1-Ethenyl-2-pyrrolidinone homopolymer [9003-39-8] Empirical Formula and Molecular Weight: (C6H9NO)n 2500–3 000 000
Spectrophotometric techniques UV spectrophotometric estimation of DOX is possible due to the presence of polyhydroxyanthraquinone chromophoric group on the 7,8,9,10-tetrahydronaphthacene skeleton. The drug when dissolved in ethanol (95%) shows characteristic peaks at 234 nm, 252 nm, 288 nm, 475 nm and at 530 nm (I.P 2014). Cia and coworkers reported the estimation of entrapment efficiency and drug loading capacity of polybutylcyanoacrylate magnetic loaded DOX nanoparticles (Cai et al., 2009). 2.10.2. Chromatographic
The computationally predicted various possible conformers are shown in Fig.1. The optimized molecular structure with the numbering of atoms of the title compound is shown in Fig.2. The most optimized structural parameters were also calculated by HF/ B3LYP have depicted in Table 1. Quantum chemical calculation was used for NFN to carry out the optimized geometry with the Gaussian 03W program [10] using the B3LYP and HF functional [11, 12] supplemented with standard 3-21G* basis set. Density Functional Theory (DFT) can be used to calculate an accurate electronic structure, HOMO and LUMO energies, Mulliken charge of atoms, energetic orbital levels, global hardness, chemical potential and electrophilicity of systems, and finally chemical, physical properties of fullerene and fullerene derivatives.
Computational Methods Of all the possible conformations of L-proline, only four can exist at ambient temperature,3, 33 and we chose the two most stable conformers for this study. The chosen conformers differ only in the puckering of pyrolidine ring of L-proline which is syn with the carboxyl group (Fig. 1a) in one conformer and anti to it (Fig. 1b) in the other. In the both chosen conformers the carboxylate group twisted toward the imino group. This geometry allows the possibility of intramolecular hydrogen bonding between the hydroxyl and the imino group of the pyrrolidine ring.
Heterocyclic chemistry comprises at least half of all organic chemistry research worldwide. Quinazolinones are the versatile nitrogen containing heterocyclic compounds. Earlier it is known as benzo-1,3-diazine and was first prepared in laboratory by Gabriel in1903 and first isolated from the chinese plant aseru.1 The name quinazoline (German : Chinazolin) was first prepared by Weddige, on observing that this was isomeric with the compounds cinnoline and quinoxaline. Paal and Bush suggested the numbering of quinazoline ring system, which is currently used.2 Quinazolinones will be classified into the following five categories based on the substitution patterns of the ring system.3 • 2-substituted-4(3H)-quinazolinones • 3-substituted-4(3H)-quinazolinones
23 atoms, 0 bonds, 0 polyhedra – that’s all this little crystal of Atheneite study of L. Bindifrom Florence U. has to offer for week #39 of this short tour of Geometry of Nature. Atheneite is a rare mineral associated with palladium-gold deposits. It is so small, it was only first identified in Brazil in 1972. Today, tiny samples can be seen at the Natural History Museum in London.
Fluorite has the capacity to increase fluidity. It reaches the melting point at 136 C. This qualities were first mentioned in 1530, by (Georgius Agricola in his work on Metals). Luster is vitreous; Transparency is crystals are transparent to translucent. Crystal system is isometric 4/m bar 3 2/m. Crystal habits includes the typical cube and to a lesser extent, the octahedron as well as combinations of these two and other rare r isometric habits. Always with equant crystals; less common are crusts and botryoidal forms.