773851-07-3

Questions And Answer

• Synthesis

  The mixture of 13.4 mg (0.046 mmol) of 2-azido-5- iodobenzoic acid and 25.8 mg (0.46 mmol) of potassium hydroxide in 10 mL of  ethanol was irradiated for 1.5 h. The reaction mixture was added to 100 mL of water containing 0.1 mL phosphoric acid and the mixture was extracted with benzene. The  benzisoxazole-containing organic phase was eluted through silica gel using benzene. The benzisoxazole-containing solution was evaporated to dryness in vacuo affording  5-iodo-2,1-benzisoxazole-3(1H)-one with 51% yield as white crystals. m/z (rel,  intensity) 261.90(11.16), 260.92(M+ , 100.00), 260.22(11.73), 259.34(8.10),  235.00(5.59), 216.96(M+-CO2, 34.90), 216.01(4.26), 134.21(6.31), 130.37(5.46),  129.09(4.35), 126.99(6.76), 90.08(26.07), 78.16(8.82), 77.07(7.23), 63.15(9.58).;