4-氯-2-碘苄醇

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: (4-Chloro-2-iodophenyl)methanol (4.67 g, 17 mmol) and PPh3 (6 mL, 26 mmol) were stirred in Et2O at 0° C. Diisopropyl azodicarboxylate (5 mL, 26 mmol) was added dropwise, and the reaction was stirred for 20 minutes (a white precipitate formed). A solution of acetone cyanohydrin (2 mL, 26 mmol) in diethyl ether (5 mL) was added dropwise to the reaction. The resulting solution was stirred for 5 minutes at 0° C. and then allowed to warm to room temperature over two hours. The reaction was monitored by TLC and LCMS. The mixture was filtered, and the filtrate was concentrated in vacuo. Purification was done using silica flash chromatography with a gradient of 0-15% EtOAc/hexanes. MS m/e=278 (M+H)+. formed) The resulting solution was stirred for 5 minutes at 0° C. The mixture was filtered the filtrate was concentrated in vacuo Purification

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

实验步骤: 4-Chloro-2-iodobenzoic acid (5.0 g, 18 mmol) was dissolved in THF (40 mL) and cooled to 0° C. Borane-THF complex (1M in THF) (35 mL, 35 mmol) was added by syringe. The solution was allowed to warm to room temperature and stirred overnight. The reaction was monitored by LCMS and TLC. When the reaction was complete, water was added until gas evolution ceased and then the THF was removed under vacuum. EtOAc (100 mL) was added, and the organic layer was washed with water (3×50 mL), brine (3×50 mL), dried with MgSO4, and concentrated in vacuo resulting in a white solid. to warm to room temperature the THF was removed under vacuum EtOAc (100 mL) was added the organic layer was washed with water (3×50 mL), brine (3×50 mL) dried with MgSO4 concentrated in vacuo resulting in a white solid

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

实验步骤: (4-Chloro-2-iodophenyl)methanol (4.67 g, 17 mmol) and PPh3 (6 mL, 26 mmol) were stirred in Et2O at 0° C. Diisopropyl azodicarboxylate (5 mL, 26 mmol) was added dropwise, and the reaction was stirred for 20 minutes (a white precipitate formed). A solution of acetone cyanohydrin (2 mL, 26 mmol) in diethyl ether (5 mL) was added dropwise to the reaction. The resulting solution was stirred for 5 minutes at 0° C. and then allowed to warm to room temperature over two hours. The reaction was monitored by TLC and LCMS. The mixture was filtered, and the filtrate was concentrated in vacuo. Purification was done using silica flash chromatography with a gradient of 0-15% EtOAc/hexanes. MS m/e=278 (M+H)+. formed) The resulting solution was stirred for 5 minutes at 0° C. The mixture was filtered the filtrate was concentrated in vacuo Purification

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

实验步骤: 4-Chloro-2-iodobenzoic acid (5.0 g, 18 mmol) was dissolved in THF (40 mL) and cooled to 0° C. Borane-THF complex (1M in THF) (35 mL, 35 mmol) was added by syringe. The solution was allowed to warm to room temperature and stirred overnight. The reaction was monitored by LCMS and TLC. When the reaction was complete, water was added until gas evolution ceased and then the THF was removed under vacuum. EtOAc (100 mL) was added, and the organic layer was washed with water (3×50 mL), brine (3×50 mL), dried with MgSO4, and concentrated in vacuo resulting in a white solid. to warm to room temperature the THF was removed under vacuum EtOAc (100 mL) was added the organic layer was washed with water (3×50 mL), brine (3×50 mL) dried with MgSO4 concentrated in vacuo resulting in a white solid