tert-Butyl hydroperoxide → 3,5,5-TRIMETHYL-3-(t-BUTYLPEROXY)CYCLOHEXANONE

HRID 1577969

반응식

HRID 1577969 반응식
[O:1]=[C:2]1[CH2:9][C:6]([CH3:8])([CH3:7])[CH2:5][C:4]([CH3:10])=[CH:3]1.[C:11]([O:15][OH:16])([CH3:14])([CH3:13])[CH3:12]>>[CH3:10][C:4]1([O:16][O:15][C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:5][C:6]([CH3:8])([CH3:7])[CH2:9][C:2](=[O:1])[CH2:3]1

참가 물질

3

반응물 2

HCID 6410tert-Butyl hydroperoxideHCID 6544Isophorone

생성물 1

HCID 205704733,5,5-TRIMETHYL-3-(t-BUTYLPEROXY)CYCLOHEXANONE

실험 절차

A reaction mixture of 62.2 g. (0.45 mole) of isophorone, 104 g. (0.9 mole) of 78% t-butyl hydroperoxide and 32.4 g. of Amberlyst 15® sulfonic acid type ion-exchange resin was stirred at 40° C. for 48 hours and at 50° C. for one hour. The ion-exchange resin was separated by filtration, the filtrate diluted with pentane and the pentane solution washed with water and sodium bisulfite solution. After drying over anhydrous magnesium sulfate, the pentane was removed under reduced pressure. The recovered product weighed 74.7 g. (72.8% of the calculated amount). The infrared spectrum had a strong absorption band in the 880 cm-1 region usually associated with t-butylperoxy groups. Iodometric assay showed the presence of active oxygen.

후처리

  1. additionA reaction mixture of 62.2 g
  2. customThe ion-exchange resin was separated by filtration
  3. additionthe filtrate diluted with pentane
  4. washthe pentane solution washed with water and sodium bisulfite solution
  5. dry with materialAfter drying over anhydrous magnesium sulfate
  6. customthe pentane was removed under reduced pressure

출처 및 근거

ORD 기록
ord-90089c7fa0bf46ef96d44bf9828b0a2d
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04289914

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