反应 #2004199
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07323604B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Prepared according to the general procedure from isophorone (138 mg, 1.09 mmol) in 0.2 M Et2O for 48 h at room temperature to provide the title compound as a colorless oil (100 mg, 65% yield, 97% ee) after purification by flash chromatography on silica gel (5% Et2O/pentane). The physical data were identical in all respects to those previously reported (Allinger et al. (1975), J. Org. Chem. 40:1316 (reported a rotation of +20.3° for the (S)-enantiomer that is 75% ee)). The enantiomeric ratio was determined by GLC using a Hydrodex-B-TBDAc (50 m×0.25 mm) column (110° C. isotherm, 1 mL/min.); (S) isomer tr=11.8 min. and (R) isomer tr=12.4 min. [α]D22=−18.7°(c=1.03, CHCl3). Prepared
来源 ID: ord-05e8d295024942b1b75b3d2a7d21a11f