反应 #1462451
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07488747B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1.6 M Methyl lithium (17.8 mL, 24.9 mmol) was added over 1 hour to a stirring 0° C. solution of (S)-3-Phenylbutyric acid (2.0147 g, 12.18 mmol) in dry Et2O (61 mL, 0.2 M): The ice bath was removed, and the reaction was allowed to stir at room temperature for 1½ additional hours. The reaction was then poured into rapidly stirring ice water containing aq. HCl. The organic layer was removed, washed with NaHCO3 and brine, then dried with Na2SO4, filtered and concentrated to achieve pure 77 (2.0487 g, (2.0487 g,˜100%): HPLC: 10.081 min. (Note: SM has HPLC retention time of 9.127 min.) The ice bath was removed The reaction was then poured into rapidly stirring ice water containing aq. HCl The organic layer was removed washed with NaHCO3 and brine dried with Na2SO4 filtered concentrated 10.081 min. (Note: SM has HPLC retention time of 9.127 min.)
来源 ID: ord-4b52e78d59a845e8ad569efdfd1dc780