反应 #1192603
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08940722B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a stirred solution of compound 31c (25.0 g, 90 mmol) in toluene-DCM (4:1, 1000 mL) was added dropwise a solution of DIBAL-H in toluene (1.0 M, 179 mL, 179 mmol) at −78° C. under argon and the mixture was stirred for 1 h at this temperature. Methanol (200 mL) was added immediately to quench the reaction. The reaction mixture was poured into a solution of 200 mL of 20% sodium potassium tartrate (Rochelle salt) and stirred at rt until the two layers separated. The organic layer was concentrated in vacuo and the residue was purified by CC (hexane/EA=2:1) to give compound 31d as a white solid (19.9 g, 89% yield). to quench the reaction stirred at rt until the two layers separated The organic layer was concentrated in vacuo the residue was purified by CC (hexane/EA=2:1)
来源 ID: ord-b8132475168d47799b0336f2c18ad427