反应详情

温度

80 °C

A mixture of spiro[isobenzofuran-1(3H),4′-piperidine]-3-one hydrochloride (40 mg), phenyl N-[5-(3-hydroxyphenyl)-2-pyrazinyl]carbamate (51 mg) and triethylamine (119 μL) in chloroform (5 mL) was stirred at 80° C. for 2 hours. The reaction mixture was poured into water and extracted with chloroform (20 mL). The organic layer was washed with saturated saline solution (20 mL) and then dried over anhydrous Na2SO4. The concentration of the solvent left a residue, which was purified by column chromatography on silica gel (hexane/ethyl acetate=4/1 to 1/2) followed by recrystallization from ethyl ether-hexane to give the subject compound (24 mg) as colorless crystals (melting point 257-259° C.).

1. extractionextracted with chloroform (20 mL)
2. washThe organic layer was washed with saturated saline solution (20 mL)
3. dry with materialdried over anhydrous Na2SO4
4. waitThe concentration of the solvent left a residue, which
5. customwas purified by column chromatography on silica gel (hexane/ethyl acetate=4/1 to 1/2)
6. customfollowed by recrystallization from ethyl ether-hexane