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With lithium aluminium tetrahydride; In tetrahydrofuran; at 0℃; for 16h;
To a solution of 4-chloro-2-fluorobenzoic acid (300mg) in THF (15m1) was added at 0CLiAIH4 (130mg). The suspension was stirred at 0C for 16h. The reaction mixture wasdiluted with EA and aq. solution of potassium sodium tartrate and stirred for lh at rt. The layers were separated and the org. phase was further washed with water. The combined org. layers were dried over MgSO4, filtrated off and evaporated in vacuo. The crude was purified by CC (Buechi Sepacore, 5g cartridge, solvent A: DCM, solvent B: 3N ammonia in MeOH, gradient in %B: 0 to 5, flow rate: 6.0 mI/mm) to afford 224mg of colourless oil. LCMS: (A) tR = 0.68 mm; [M+H]: not visible.
224 mg
With lithium aluminium tetrahydride; In tetrahydrofuran; at 0℃; for 16h;Inert atmosphere;
To a solution of 4-chloro-2-fluorobenzoic acid (300 mg) in THF (15 ml_) was added at 0C UAIH4 (130 mg). The suspension was stirred at 0C for 16h. The reaction mixture was diluted with EA and aq. solution of potassium sodium tartrat and stirred for 1 h at rt. The layers were separated and the org. phase was further washed with water. The combined org. layers were dried over MgS04, filtrated off and evaporated in vacuo. The crude was purified by CC (Buchi Sepacore, 5g cartridge, solvent A: DCM, solvent B: 3N ammonia in MeOH, gradient in %B: 0 to 5, flow rate: 6.0 imL/min) to afford 224 mg of colourless oil. LC-MS (A) tR = 0.68 min; [M+H]+: not visible.
224 mg
With lithium aluminium tetrahydride; In tetrahydrofuran; at 0℃; for 16h;
To a solution of 4-chloro-2-fluorobenzoic acid (300mg) in THF (15ml) was added at 0C UAIH4 (130mg). The suspension was stirred at 0C for 16h. The reaction mixture was diluted with EA and aq. solution of potassium sodium tartrat and stirred for 1 h at rt. The layers were separated and the org. phase was further washed with water. The combined org. layers were dried over MgS04, filtrated off and evaporated in vacuo. The crude was purified by CC (Buchi Sepacore, 5g cartridge, solvent A: DCM, solvent B: 3N ammonia in MeOH, gradient in %B: 0 to 5, flow rate: 6.0 ml/min) to afford 224mg of colourless oil. LC-MS (A) tR = 0.68min; [M+H]+: not visible.
With copper (II) nitrate tetrahydrate; oxygen; In acetonitrile; at 180℃; under 18751.9 Torr; for 1.5h;Green chemistry;
<strong>[175711-83-8]2-fluoro-4-chloroacetophenone</strong> 25g (144.9mmol, 1.0eq), Cu(NO3)2·4H2O 7.0g (29.0mmol, 0.2eq), acetonitrile 250mL (10V),The temperature of the outer bath of the reaction coil was raised to 180 C, and the coil pressure was adjusted to 2.5 MPa with oxygen to start the charging. The residence time of the system was 1.5 h and the oxygen was 3 to 5 eq.The system was directly pumped into 375 mL of purified water, and the pH of the system was adjusted to 12-14 with NaOH solids.The aqueous phase was extracted twice with 125 mL MTBE, and the aqueous phase was adjusted to pH 1 with concentrated HCl.A large amount of solid was precipitated, and 19.3 g of the target product was obtained by filtration, yield 77%.
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