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34047180926
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General Procedure for Liquid Nitriles A mixture of 50 mmol of nitrile, silica sulfuric acid (0.18 g, equal to 1.36 mmol H, and 1 mmol of carboxylic anhydride was heated in a 25 mL round-bottomed flask at 60-70°C The reactions were completed within 6-8 h as monitored by TLC (eluent, EtOAc-PE, 1:1, The mixture was filtered and solvent was evaporated under reduced pressure. A solution of NaHCO3 in H2O (1, 10 mL) was added and the mixture was extracted with Et2O (3 x 25 mL, The organic layer was separated and dried over Na2SO4. When necessary, the crude product was purified by preparative TLC on silica gel. General Procedure for Solid Nitriles In a round-bottomed flask the solid nitrile (1 mmol, carboxylic anhydride (1 mmol) and silica sulfuric acid 0.18 g, equal to 1.36 mmol H, were mixed thoroughly. The flask was heated at 40-50°C with concomitant stirring. After completion of the re
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+) were mixed thoroughly. The flask was heated at 40-50°C with concomitant stirring. After completion of the reaction confirmed by TLC (eluent: EtOAc-PE, 1:9), EtOAc (15 mL) was added and filtered. The filtrate was concentrated and purified by preparative TLC.
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+], 162 (30), 119 (100), 91 (80), 65 (52).
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