反应详情

To a solution of (S)-pyrrolidine-2-carboxylic acid (5-tert-butyl-isoxazol-3-yl)-amide; hydrochloride (0.150 g; 0.580 mmol) in N,N-dimethylformamide (2 mL) is added 4-chlorophenylsulfonyl chloride (0.122 g; 0.580 mmol) and triethylamine (0.243 mL; 1.740 mmol). The mixture is stirred at room temperature overnight. After this time, the mixture is diluted with water and extracted with ethyl acetate. The combined organics are washed with aqueous saturated sodium bicarbonate solution, 1N hydrochloric acid, and brine, dried (Na2SO4), filtered and concentrated in vacuo. The crude material is purified by preparative HPLC to afford title compound. ESI m/z 412 [M+NH4]+

1. extractionextracted with ethyl acetate
2. washThe combined organics are washed with aqueous saturated sodium bicarbonate solution, 1N hydrochloric acid, and brine
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude material is purified by preparative HPLC