反应详情

温度

0 °C

4-Aminoantipyrine (0.12 mmol, Aldrich) and octachloro-octachloro tetrasulfonato Fe(III) porphyrin (0.6 μmol) were dissolved in 4 ml of pH 7 phosphate buffer and cooled to 0° C. To this was added iodosobenzene (66 mg, 0.3 mmol) was added in portions over 10 min. The reaction was stirred for 4 hr and extracted with 3×2 ml of methylene chloride and dried over Na2CO3. The organic layer was chromatographed over silica gel, eluting with methylene chloride, to yield 2,3-dimethyl-4-hydroxyamino-1-phenyl-3-pyrazolin-5-one (AP-3) in 30% yield.

1. additionwas added in portions over 10 min
2. extractionextracted with 3×2 ml of methylene chloride
3. dry with materialdried over Na2CO3
4. customThe organic layer was chromatographed over silica gel
5. washeluting with methylene chloride