反应详情

Nanosized activated iron powder in mineral oil (0.042 g) is rinsed successively with two 2 ml portions of cyclohexane. Most of the solvent is removed with a pipette. The iron is added to a mixture of 5.00 g (29.0 mmol) of 1-oxyl-2,2,6,6-tetramethylpiperidin-4-ol, 44 ml of acetonitrile, and 32 ml of cyclohexane that has been heated to 40 degrees. To this mixture is carefully added over several minutes a solution of 0.548 g of concentrated hydrochloric acid in 3 ml of water. The reaction temperature is brought to reflux and a solution of 7.81 g (115 mmol) of 50% aqueous hydrogen peroxide is added dropwise over a period of 2.25 hours. After about one-half of the peroxide solution is added, a second portion of nanosized activated iron powder in mineral oil (0.039 g), rinsed twice with cyclohexane, and a solution of 0.166 g of concentrated hydrochloric acid in 1 ml of water are added to the reaction mixture. The reaction mixture is heated at 60-62 degrees for 1.5 hours after the peroxide has been added. After work up and purification according to the procedure of Example 54, the yield of the title compound is 5.53 g (75% yield), GC assay 96%.

1. washNanosized activated iron powder in mineral oil (0.042 g) is rinsed successively with two 2 ml portions of cyclohexane
2. customMost of the solvent is removed with a pipette
3. temperaturehas been heated to 40 degrees
4. temperatureto reflux
5. washa second portion of nanosized activated iron powder in mineral oil (0.039 g), rinsed twice with cyclohexane
6. additiona solution of 0.166 g of concentrated hydrochloric acid in 1 ml of water are added to the reaction mixture
7. temperatureThe reaction mixture is heated at 60-62 degrees for 1.5 hours after the peroxide
8. additionhas been added
9. customAfter work up and purification