反应详情

A 100 mL vessel was charged with 1,1-dioxothietan-3-amine hydrochloride (1.2 g) in 25 mL of N,N-dimethylformamide followed by successive addition of triethylamine (2.1 mL), hydroxyazabenzotriazole (1 g), 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide (1.4 g) and 4-[(5S)-5-(3,5-dichloro-4-fluoro-phenyl)-5-(trifluoromethyl)-4H-isoxazol-3-yl]-2-methyl-benzoic acid (2.6 g) dissolved in N,N-dimethylformamide (5 mL). The mixture was then stirred overnight at room temperature. The reaction mixture was diluted in 600 mL of ethyl acetate, washed 3-times with 500 mL of brine, then with 0.5N HCl cold, dried over MgSO4 and evaporated to yield 4.6 g of the crude title compound. The product was purified over a silica gel column (eluent: CH2Cl2/EtOAc) to yield 2 g of the title compound.

1. washwashed 3-times with 500 mL of brine
2. dry with materialwith 0.5N HCl cold, dried over MgSO4
3. customevaporated
4. customto yield 4.6 g of the crude title compound
5. customThe product was purified over a silica gel column (eluent: CH2Cl2/EtOAc)