反应 #1648492
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08318830B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 10 g (39 mmol) of benzoylbenzoic ethylester are added to a suspension of 3.94 g (35 mmol) of potassium-tert-butoxid in 60 ml of THF at 0° C. under argon. 2.82 g (33 mmol) of 3-methyl-2-butanone are added in 1 h while the temperature rises to 25° C. After 2 h at 40° C. the reaction mixture is poured into 500 ml of ice water containing 10 ml conc. HCl. Extraction with toluene and evaporation gives the crude product (8.5 g) which is purified by crystallisation in heptane yielding 3.7 g of a white solid. The structure is confirmed by 1H-NMR and 13C-NMR spectra. mp: 76.5-78° C. rises to 25° C Extraction with toluene and evaporation
来源 ID: ord-68b8389eaf4b4f6dbfe03b8110b546cd