Hydrogen Peroxide → 1-Cyclohexyloxy-4-benzoyloxy-2,2,6,6-tetramethylpiperidine

HRID 133647

反応式

HRID 133647 の反応式
[OH:1][N:2]1[C:7]([CH3:9])([CH3:8])[CH2:6][CH:5]([O:10][C:11](=[O:18])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:4][C:3]1([CH3:20])[CH3:19].C(#N)C.[CH2:24]1[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1.OO>O>[CH:24]1([O:1][N:2]2[C:7]([CH3:9])([CH3:8])[CH2:6][CH:5]([O:10][C:11](=[O:18])[C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:4][C:3]2([CH3:20])[CH3:19])[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1

参加物

6

反応物 4

HCID 784Hydrogen PeroxideHCID 6342AcetonitrileHCID 8078CyclohexaneHCID 6881781-Hydroxy-4-benzoyloxy-2,2,6,6-tetramethylpiperidine

生成物 1

HCID 233720981-Cyclohexyloxy-4-benzoyloxy-2,2,6,6-tetramethylpiperidine収率 84%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
56 °C

実験手順

A solution of 0.097 g (0.359 mmol) of ferric chloride hexahydrate in 2 ml of water is added to a mixture of 5.00 g (18.1 mmol) of 1-oxyl-4-benzoyloxy-2,2,6,6-tetramethylpiperidine, 28 ml of acetonitrile, and 19 ml of cyclohexane. The mixture is heated to 56° C. A solution of 4.70 g (69 mmol) of 50% aqueous hydrogen peroxide is added dropwise over 2.25 hours to the reaction mixture while the temperature is brought to and maintained at reflux. After the peroxide is added, the mixture is heated at reflux for 45 minutes. Work-up and purification according to the procedure of Example 5 afford 5.47 g (84% yield) of the title compound, a pale yellow syrup. GC assay is 100%.

後処理

  1. temperaturemaintained
  2. temperatureat reflux
  3. temperaturethe mixture is heated
  4. temperatureat reflux for 45 minutes
  5. customWork-up and purification

出典と根拠

ORDレコード
ord-08c14529a5624a229bb297bff01f9af8
出典データセット
uspto-grants-2008_06
特許番号
US07390904B2

関連ノート

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