反应详情

Ammonium chloride (3.23 g), 1-hydroxybenzotriazole (2.45 g), IPEA (13.7 mL) and benzotriazol-1-yloxytris(pyrrolidino)phosphonimn hexafluorophosphate (9.43 g) were sequentially added to a solution of 5-chloro-2-(4-chloro-2-trifluoromethylphenyl)pentanoic acid (4.75 g) in N,N-dimethylformamide (45 mL). The mixture was stirred at room temperature overnight. Ice water and tert-butyl methyl ether were added to the reaction solution, and the organic layer was separated. The aqueous layer was reextracted with tert-butyl methyl ether. The combined organic layers were sequentially washed with 1 N hydrochloric acid, water, a saturated sodium bicarbonate aqueous solution and brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (carrier: Wakogel™ C-200; elution solvent:heptane:ethyl acetate=4:1→3:1) to obtain 3.89 g of the title compound. The property values of the compound are as follows.

1. customthe organic layer was separated
2. washThe combined organic layers were sequentially washed with 1 N hydrochloric acid, water
3. dry with materiala saturated sodium bicarbonate aqueous solution and brine, dried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe resulting residue was purified by silica gel column chromatography (carrier: Wakogel™ C-200; elution solvent:heptane:ethyl acetate=4:1→3:1)