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Asymmetric Copper-Catalyzed Addition of Grignard Reagents to Aryl Alkyl Ketones**
| Content Provider | CiteSeerX |
|---|---|
| Author | Madduri, Ashoka V. R. Harutyunyan, Syuzanna R. Minnaard, Adriaan J. |
| Abstract | visualized by UV and Seebach’s reagent, a mixture of phosphomolybdic acid (25 g), cerium (IV) sulfate (7.5 g), H2O (500 mL) and H2SO4 (25 mL) or potassium permanganate staining. Progress and conversion of the reaction were determined by GC-MS (GC, HP6890: MS HP5973) with an HP1 or HP5 column (Agilent Technologies, Palo Alto, CA). High resolution mass spectra (HRMS) were recorded on a AEI-MS-902 and FTMS orbitrap (Thermo Fisher Scientific) mass spectrometer. 1H- and 13C-NMR were recorded on a Varian AMX400 (400 and 100.59 MHz, respectively) or a Varian Gemini 200, using CDCl3 as solvent. Chemical shift values are reported in ppm with the solvent resonance as the internal standard (CHCl3: δ 7.26 for 1H, δ 77.0 for 13C). Data are reported as follows: chemical shifts, multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, br = broad, m = multiplet), coupling constants (Hz), and integration. Carbon assignments are based on APT 13C-NMR experiments. Optical rotations were measured on a Schmidt + Haensch polarimeter (Polartronic MH8) with a 10 cm cell (c given in g/100 mL). Enantiomeric excesses were determined by HPLC analysis using a Shimadzu LC-10ADVP HPLC equipped with a Shimadzu SPD-M10AVP diode array detector or by capillary GC analysis (HP 6890, CP-Chiralsil-Dex-CB column (25 m x 0.25 mm) or Chiraldex B-PM (30 m x 0.25 mm x 0.25 µm)) using a flame ionization detector. All reactions were carried out under a nitrogen atmosphere using oven dried glassware and using standard Schlenk techniques. tBuOMe and dichloromethane were dried and distilled from calcium hydride; toluene, THF and n-hexane were dried and distilled from sodium. All copper salts were purchased from Aldrich, and used without further purification. All |
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| Access Restriction | Open |
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