2-(2-溴-4-氟苯基)丙-2-醇

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

实验步骤: Add 98% sulfuric acid drop-wise (3 g, 31 mmol) to a mixture of 2-(2-bromo-4-fluoro-phenyl)-propan-2-ol (2.4 g, 10.30 mmol) and trimethylsilyl cyanide (2.04 g, 59 mmol) in a 25-mL round bottom flask under N2 at −20° C. Move the flask out of the cooling bath and stir the mixture at RT overnight. Dilute the mixture with ice-water and neutralize with ammonium hydroxide to pH=8. Extract the product with chloroform/IPA (3/1, 100 mL). Wash the organic phase with water/aqueous saturated sodium chloride, dry over sodium sulfate, and concentrate in vacuo to give the crude product. Purify by FCC (20% THF in DCM as elute) to give the title compound as a white solid (2 g, 75%). MS (ES) m/z 260/262 [M+1]+. Extract the product with chloroform/IPA (3/1, 100 mL) Wash the organic phase with water/aqueous saturated sodium chloride dry over sodium sulfate concentrate in vacuo to give the crude product Purify by FCC (20% THF in DCM as elute)

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

实验步骤: Add 98% sulfuric acid drop-wise (3 g, 31 mmol) to a mixture of 2-(2-bromo-4-fluoro-phenyl)-propan-2-ol (2.4 g, 10.30 mmol) and trimethylsilyl cyanide (2.04 g, 59 mmol) in a 25-mL round bottom flask under N2 at −20° C. Move the flask out of the cooling bath and stir the mixture at RT overnight. Dilute the mixture with ice-water and neutralize with ammonium hydroxide to pH=8. Extract the product with chloroform/IPA (3/1, 100 mL). Wash the organic phase with water/aqueous saturated sodium chloride, dry over sodium sulfate, and concentrate in vacuo to give the crude product. Purify by FCC (20% THF in DCM as elute) to give the title compound as a white solid (2 g, 75%). MS (ES) m/z 260/262 [M+1]+. Extract the product with chloroform/IPA (3/1, 100 mL) Wash the organic phase with water/aqueous saturated sodium chloride dry over sodium sulfate concentrate in vacuo to give the crude product Purify by FCC (20% THF in DCM as elute)