反应 #2997805
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08063035B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Add trimethylsilyl cyanide (1.01 mL, 7.39 mmol) and zinc diiodide (0.11 g, 0.37 mmol) to a solution of 2-bromo-4-fluorobenzaldehyde (1.5 g, 7.39 mmol) in DCM (10 mL). Stir the mixture overnight at RT. Remove the solvent. Dissolve the residue in THF (5 mL) and cool at 0° C. Add borane-THF complex (11.1 mL, 11.1 mmol). Stir the mixture at RT for 3 h. Add 1 M HCl slowly and stir for 15 min. Adjust the pH to basic with saturated sodium carbonate. Extract with DCM. Dry it over sodium sulfate and concentrate to give the title compound as a colorless oil (1.5 g, 86%). MS (ES) m/z 235 [M+1]+. Remove the solvent Dissolve the residue in THF (5 mL) cool at 0° C Stir the mixture at RT for 3 h stir for 15 min Extract with DCM Dry it over sodium sulfate concentrate
来源 ID: ord-1bf30752434d4c91a9023986a67364ee