反应详情

温度

75 °C

To a solution of 4-[5-(3,5-Dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-2-methyl-benzaldehyde oxime (i.e. the product of Step 2, 500 mg) in DMF (25 mL) was added N-chloro succinimide (168 mg) and heated to 75° C. for 1 h. After cooling, the reaction mixture was poured onto water and extracted with MTBE. The combined organic layers were dried (Na2SO4) and concentrated in vacuo to ¼ of the original volume to obtain the crude hydroxamic acid chloride. This mixture was added to a solution of methylamine (0.66 mL, 41 mg) and triethylamine (0.18 mL, 0.13 g) in THF and stirred at room temperature over night. After concentration in vacuo, the mixture was purified by chromatography on silica gel to obtain the title compound (270 mg, 39%) as a colorless solid.

1. temperatureAfter cooling
2. additionthe reaction mixture was poured onto water
3. extractionextracted with MTBE
4. dry with materialThe combined organic layers were dried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customto obtain the crude hydroxamic acid chloride
7. concentrationAfter concentration in vacuo
8. customthe mixture was purified by chromatography on silica gel