反应 #1713924
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08389511B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: (S)-3,3,3-Trifluoro-2-hydroxy-2-methylpropionic acid (1.00 g) was dissolved in tetrahydro-furan (10.0 ml), and thereto were added successively benzotriazol-1-yl-oxy-tris-pyrrolidino-phosphonium hexafluorophosphate (3.64 g) and triethylamine (1.80 ml) under ice-cooling, and the mixture was stirred at room temperature. Ten hours later, to the reaction solution was added a 1N aqueous hydrochloric acid solution under ice-cooling, and the mixture was extracted with ethyl acetate. The organic layer was washed successively with a saturated aqueous sodium hydrogen carbonate solution and a saturated aqueous sodium chloride solution, dried over sodium sulfate, filtered and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (the developing solvent: hexane/ethyl acetate=10/1, 5/1) to give the title compound (1.10 g) as a colorless liquid. cooling cooling the mixture was extracted with ethyl acetate The organic layer was washed successively with a saturated aqueous sodium hydrogen carbonate solution a saturated aqueous sodium chloride solution, dried over sodium sulfate filtered concentrated under reduced pressure The obtained residue was purified by silica gel column chromatography (the developing solvent
来源 ID: ord-c787be264e9c4cdd89ba41303c495c5c