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

HRID 133647

반응식

HRID 133647 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 233720981-Cyclohexyloxy-4-benzoyloxy-2,2,6,6-tetramethylpiperidine수율 84%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
56 °C

실험 절차

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%.

후처리

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

출처 및 근거

ORD 기록
ord-08c14529a5624a229bb297bff01f9af8
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07390904B2

연결된 노트

불러오는 중…