反应 #3505852
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08138175B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 2.48 g (10.00 mmol) of methyl (S)-4-(tert-butyldimethylsilyloxy)-2-hydroxybutanoate (J. Am. Chem. Soc. 2005 127, 1090-1091) in 50 ml of CH2Cl2 was treated with 2.09 ml (15.00 mmol, 1.5 eq) of triethylamine and at 0° C. during 5 min with 0.82 ml (10.50 mmol, 1.051 eq) of methanesulfonyl chloride. After 1 h at 0° C. the reaction was partitioned between 10% aq KH2PO4/Et2O (×3), the organic phases were washed with sat. aq. NaHCO3 solution (freshly prepared) and 10% aq. NaCl solution, dried over Na2SO4 and evaporated to give 2.91 g (89%) of the title compound as yellow oil. MS: 327.1 (MH+). After 1 h at 0° C. the reaction was partitioned between 10% aq KH2PO4/Et2O (×3) the organic phases were washed with sat. aq. NaHCO3 solution ( freshly prepared) and 10% aq. NaCl solution dried over Na2SO4 evaporated
来源 ID: ord-635dbd1093c14e1daf9868942734c81f