tert-Butyl hydroperoxide → 2,6-DIMETHYL-2,6-bis(t-BUTYLPEROXY)-4-HEPTANONE

HRID 1577967노트

반응식

HRID 1577967 반응식
[CH3:1][C:2](=[CH:4][C:5](=[O:10])[CH:6]=[C:7]([CH3:9])[CH3:8])[CH3:3].[C:11]([O:15][OH:16])([CH3:14])([CH3:13])[CH3:12]>>[CH3:1][C:2]([O:16][O:15][C:11]([CH3:14])([CH3:13])[CH3:12])([CH2:4][C:5](=[O:10])[CH2:6][C:7]([CH3:9])([O:16][O:15][C:11]([CH3:14])([CH3:13])[CH3:12])[CH3:8])[CH3:3]

참가 물질

3

반응물 2

HCID 6410tert-Butyl hydroperoxideHCID 10438Phorone

생성물 1

HCID 205704682,6-DIMETHYL-2,6-bis(t-BUTYLPEROXY)-4-HEPTANONE

실험 절차

A mixture of 47.0 g. (0.34 mole) of phorone and 157 g (1.36 mole) of 78% t-butyl hydroperoxide was stirred with 34 g. of dry Amberlyst 15® sulfonic acid type ion exchange resin in a 500 ml flask equipped with a condenser and thermometer for forty-eight hours at 40° C. and one hour at 50° C. The ion exchange resin was separated by filtration and the product diluted with pentane. The pentane solution was washed with water, sodium bisulfite solution, 5% sodium hydroxide solution and water. After drying over anhydrous magnesium sulfate, the pentane was removed under reduced pressure. The recovered product weighed 74.2 g. (68.5% of the calculated amount). A GLC scan showed a large major peak for the expected product. In the infrared spectrum, small bands for hydroxyl and olefin were observed but the band in the 880 cm-1 region usually associated with t-butyl peroxy groups was strong. By active oxygen assay, the purity of the products was estimated at 83%.

후처리

  1. additionA mixture of 47.0 g
  2. customThe ion exchange resin was separated by filtration
  3. additionthe product diluted with pentane
  4. washThe pentane solution was washed with water, sodium bisulfite solution, 5% sodium hydroxide solution and water
  5. dry with materialAfter drying over anhydrous magnesium sulfate
  6. customthe pentane was removed under reduced pressure

출처 및 근거

ORD 기록
ord-38b4d0e2401346b8a75062daa48bce93
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04289914

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