Dry Acetonitrile Lab Report
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
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