Sulfuric Acid → 2,6-DIMETHYL-2,6-bis(t-BUTYLPEROXY)-4-HEPTANONE

HRID 127868

반응식

HRID 127868 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].S(=O)(=O)(O)O>CCCCC>[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

5

반응물 3

HCID 1118Sulfuric AcidHCID 6410tert-Butyl hydroperoxideHCID 10438Phorone

생성물 1

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

시약·촉매·용매 1

HCID 8003Pentane용매

반응 조건

온도
10 °C

실험 절차

A mixture of 6.9 g. (0.05 mole) of phorone and 23.2 g. (0.2 mole) of anhydrous 81% t-butyl hydroperoxide was diluted with 50 ml of pentane and the mixture stirred at 10° C., while 5.7 g. of 77% sulfuric acid solution was slowly added over a thirty minute time period. The mixture was then allowed to warm slowly to 25° C. and stirred for 72 hours. After the reaction mixture was washed with water and sodium bisulfite solution, it was dried over anhydrous magnesium sulfate, the drying agent separated and the pentane removed under reduced pressure. The product weighed 11.4 g. (71.7% of the calculated amount). The infrared spectrum showed a strong absorption in the 880 cm-1 region, usually associated with t-butylperoxy groups and no absorption in the regions ascribed to hydroxyl or olefin. A GLC scan showed one large major peak for the expected product. By active oxygen assay, the purity of the product was estimated at 93%.

후처리

  1. additionA mixture of 6.9 g
  2. temperatureto warm slowly to 25° C.
  3. stirringstirred for 72 hours
  4. washAfter the reaction mixture was washed with water and sodium bisulfite solution, it
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. customthe drying agent separated
  7. customthe pentane removed under reduced pressure
  8. customa strong absorption in the 880 cm-1 region
  9. customno absorption in the regions

출처 및 근거

ORD 기록
ord-5f68cb4616b74217ace280c05ada0e40
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04257985

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