2-羟基-5-碘苯甲腈

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: K2CO3 (91.0 g, 0.656 mol) was added to a solution of 2-hydroxy-5-iodo-benzonitrile (80.0 g, 0.328 mol) and 2-chloro-5-tri-fluoromethyl-pyridine (60.0 g, 0.328 mol) in DMF (500 ml) was added. The reaction mixture was refluxed overnight, filtered and concentrated. Purification via FC (PE/EtOAc=10/1) afforded the title product as a white solid (120 g). was added The reaction mixture was refluxed overnight filtered concentrated Purification via FC (PE/EtOAc=10/1)

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: CF3SO3H (40 mL) was added dropwise to a solution of 2-hydroxy-benzonitrile (47.6 g, 0.400 mmol) in CH3CN (500 mL) at 0° C., and then stirred at 0° C. for 20 min, then NIS (108 g, 0.48 mmol) was added. The reaction mixture was stirred at rt overnight, concentrated, then diluted with H2O (300 mL) and extracted with EA (300 mL×3). The combined organic parts were dried over anhydrous Na2SO4, filtered, and concentrated. Purification via FC (PE/EtOAc=5/1) afforded the title compound as a white solid (80 g). The reaction mixture was stirred at rt overnight concentrated diluted with H2O (300 mL) extracted with EA (300 mL×3) The combined organic parts were dried over anhydrous Na2SO4 filtered concentrated Purification via FC (PE/EtOAc=5/1)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-hydroxy-5-iodo-benzonitrile (80.0 g, 0.328 mol) and 2-chloro-5-tri fluoromethylpyridine (60.0 g, 0.328 mol) in DMF (500 ml) was added K2CO3 (91.0 g, 0.656 mol). The reaction mixture was refluxed overnight, then filtered and concentrated. Purification via column chromatography on silica gel (petroleum ether/ethyl acetate=10/1) afforded the title product (120 g) as a white solid. The reaction mixture was refluxed overnight filtered concentrated Purification via column chromatography on silica gel (petroleum ether/ethyl acetate=10/1)

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-hydroxy-benzonitrile (47.6 g, 0.400 mmol) in CH3CN (500 mL) was added CF3SO3H (40 mL) dropwise at 0° C. The reaction mixture was stirred at 0° C. for 20 min, and then NIS (108 g, 0.48 mmol) was added. The mixture was stirred at room temperature overnight, then concentrated, diluted with H2O (300 mL) and extracted with EA (300 mL×3). Combined organic portions were dried over sodium sulfate, filtered and reconcentrated. Purification via column chromatography on silica gel (petroleum ether/ethyl acetate=5/1) afforded the title product (80 g) as a white solid. The mixture was stirred at room temperature overnight concentrated diluted with H2O (300 mL) extracted with EA (300 mL×3) Combined organic portions were dried over sodium sulfate filtered Purification via column chromatography on silica gel (petroleum ether/ethyl acetate=5/1)

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-hydroxy-benzonitrile (47.6 g, 0.400 mmol) in CH3CN (500 mL) was added CF3SO3H (40 mL) dropwise at 0° C. The reaction mixture was stirred at 0° C. for 20 min, and then NIS (108 g, 0.48 mmol) was added. The mixture was stirred at room temperature overnight, then concentrated, diluted with H2O (300 mL) and extracted with EA (300 mL×3). Combined organic portions were dried over sodium sulfate, filtered and reconcentrated. Purification via column chromatography on silica gel (petroleum ether/ethyl acetate=5/1) afforded the title product (80 g) as a white solid. The mixture was stirred at room temperature overnight concentrated diluted with H2O (300 mL) extracted with EA (300 mL×3) Combined organic portions were dried over sodium sulfate filtered Purification via column chromatography on silica gel (petroleum ether/ethyl acetate=5/1)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: K2CO3 (91.0 g, 0.656 mol) was added to a solution of 2-hydroxy-5-iodo-benzonitrile (80.0 g, 0.328 mol) and 2-chloro-5-tri-fluoromethyl-pyridine (60.0 g, 0.328 mol) in DMF (500 ml) was added. The reaction mixture was refluxed overnight, filtered and concentrated. Purification via FC (PE/EtOAc=10/1) afforded the title product as a white solid (120 g). was added The reaction mixture was refluxed overnight filtered concentrated Purification via FC (PE/EtOAc=10/1)

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: CF3SO3H (40 mL) was added dropwise to a solution of 2-hydroxy-benzonitrile (47.6 g, 0.400 mmol) in CH3CN (500 mL) at 0° C., and then stirred at 0° C. for 20 min, then NIS (108 g, 0.48 mmol) was added. The reaction mixture was stirred at rt overnight, concentrated, then diluted with H2O (300 mL) and extracted with EA (300 mL×3). The combined organic parts were dried over anhydrous Na2SO4, filtered, and concentrated. Purification via FC (PE/EtOAc=5/1) afforded the title compound as a white solid (80 g). The reaction mixture was stirred at rt overnight concentrated diluted with H2O (300 mL) extracted with EA (300 mL×3) The combined organic parts were dried over anhydrous Na2SO4 filtered concentrated Purification via FC (PE/EtOAc=5/1)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-hydroxy-5-iodo-benzonitrile (80.0 g, 0.328 mol) and 2-chloro-5-tri fluoromethylpyridine (60.0 g, 0.328 mol) in DMF (500 ml) was added K2CO3 (91.0 g, 0.656 mol). The reaction mixture was refluxed overnight, then filtered and concentrated. Purification via column chromatography on silica gel (petroleum ether/ethyl acetate=10/1) afforded the title product (120 g) as a white solid. The reaction mixture was refluxed overnight filtered concentrated Purification via column chromatography on silica gel (petroleum ether/ethyl acetate=10/1)

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-hydroxy-benzonitrile (47.6 g, 0.400 mmol) in CH3CN (500 mL) was added CF3SO3H (40 mL) dropwise at 0° C. The reaction mixture was stirred at 0° C. for 20 min, and then NIS (108 g, 0.48 mmol) was added. The mixture was stirred at room temperature overnight, then concentrated, diluted with H2O (300 mL) and extracted with EA (300 mL×3). Combined organic portions were dried over sodium sulfate, filtered and reconcentrated. Purification via column chromatography on silica gel (petroleum ether/ethyl acetate=5/1) afforded the title product (80 g) as a white solid. The mixture was stirred at room temperature overnight concentrated diluted with H2O (300 mL) extracted with EA (300 mL×3) Combined organic portions were dried over sodium sulfate filtered Purification via column chromatography on silica gel (petroleum ether/ethyl acetate=5/1)