反应详情

4-Chloromethyl-3,5-dimethylisoxazole (700 mg, 4.8 mmol) is suspended in concentrated aqueous ammonia at 20-25 degrees C., and vigorously stirred overnight. The reaction mixture is extracted with isopropyl alcohol/chloroform (10/90, 2×). The combined organic phases are concentrated under nitrogen flow. The residue is purified by flash chromatography methanol/methylene chloride (5-20%, 1% triethylamine) to give the title compound, MR (CDCl3, 300 MHz) delta3.62, 2.37, 2.29, and 1.44.

1. customvigorously stirred overnight
2. extractionThe reaction mixture is extracted with isopropyl alcohol/chloroform (10/90, 2×)
3. concentrationThe combined organic phases are concentrated under nitrogen flow
4. customThe residue is purified by flash chromatography methanol/methylene chloride (5-20%, 1% triethylamine)