反应详情

To an ice-cooled and stirred mixture of [2-(7-ethoxy-5-{[6-(methylsulfonyl)pyridin-3-yl]oxy}-1H-indol-2-yl)-4,5-dihydro-1,3-thiazol-5-yl]acetic acid (95 mg) in N,N-dimethylformamide (5 mL) were added 1-hydroxybenzotriazole ammonium salt (61 mg) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (77 mg). After stirring at 4° C. to room temperature for 15 h, the reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed successively with aqueous sodium hydrogen carbonate solution and brine, dried (MgSO4), filtered, and concentrated to give a pale yellow amorphous solid, which was crystallized from ethyl acetate-hexane to give the title compound (84 mg) as colorless crystals. Recrystallization from ethyl acetate-hexane gave the title compound (71 mg, 76%) as colorless crystals. MS 475 (MH+). mp 195-196° C.

1. stirringAfter stirring at 4° C. to room temperature for 15 h
2. customthe reaction mixture was partitioned between ethyl acetate and water
3. washThe organic layer was washed successively with aqueous sodium hydrogen carbonate solution and brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customto give a pale yellow amorphous solid, which
8. customwas crystallized from ethyl acetate-hexane