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Experimental-Schematic Representation And Procedure For Synthesis Lab Report

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6.3 Experimental - schematic representation and procedure for the synthesis of compounds V1-17 6.3.1 Synthesis of 6-nitro-1H-benzo[d]imidazole-2-thiol II (step 1) Ethanol (40 ml) and potassium hydroxide (0.01 mol, 56.11 gm/mol, 0.56 gm in 2 ml H2O) were taken in a dry round bottom flask. 4-nitrobenzene-1,2- diamine I (0.01 mol, 153.14 gm/mol, 1.53 gm) was added to it and stirred well to get a clear solution. Carbon disulfide (0.02 mol, 76.14 gm/mol, 1.2 mL) was added to the clear solution obtained above and refluxed for 12 -15 h. The ethanol was distilled off and then cooled to room temperature. The content was poured into water and acidified with diluted HCl till the precipitates were separated. The separated solid was washed with cold water and dried to get the desired product. The completion of the reaction was monitored by TLC using ethyl acetate: …show more content…

°C % Yield Elemental Analysis % Carbon % Hydrogen %Nitrogen Calcd. Found Calcd. Found Calcd. Found V1 -H C15H12N4O3S 328 1420C 54% 54.87 54.85 03.68 03.70 17.06 17.09 V2 -4-NO2 C15H11N5O5S 373 1360C 83% 48.26 48.27 02.97 02.95 18.76 18.73 V3 -3-NO2 C15H11N5O5S 373 1400C 93% 48.26 48.29 02.97 02.99 18.76 18.75 V4 -2-NO2 C15H11N5O5S 373 1140C 92% 48.26 48.22 02.97 02.94 18.76 18.78 V5 -4-F C15H11FN4O3S 346 2100C 81% 52.02 52.06 03.20 03.23 16.18 16.15 V6 -4-Cl C15H11ClN4O3S 362 1940C 80% 49.66 49.68 03.06 03.04 15.44 15.47 V7 -3-Cl C15H11ClN4O3S 362 1820C 88% 49.66 49.63 03.06 03.08 15.44 15.42 V8 -3-Cl-4-F C15H10ClFN4O3S 380 2080C 86% 47.31 47.33 02.65 02.62 14.71 14.74 V9 -3-CF3 C16H11F3N4O3S 396 1980C 94% 48.49 48.51 02.80 02.83 14.14 14.12 6.4.1 Table-3: Physical constants data for derivatives V10-17 (Conti…) Derivatives Substituent Molecular formula Molecular weight gm/mol m.p. °C % Yield Elemental

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