Acetone → 2,2-Di-(t-Octylperoxy) Propane

HRID 1605613

반응식

HRID 1605613 반응식
[CH3:1][C:2]([CH3:4])=[O:3].[CH3:5][C:6]([O:13][OH:14])([CH3:12])[CH2:7][C:8]([CH3:11])([CH3:10])[CH3:9].S(=O)(=O)(O)O>CCCCC>[C:2]([O:3][O:13][C:6]([O:14][O:13][C:6]([CH2:7][C:8]([CH3:11])([CH3:10])[CH3:9])([CH3:12])[CH3:5])([CH3:12])[CH3:5])([CH2:7][C:8]([CH3:11])([CH3:10])[CH3:9])([CH3:4])[CH3:1]

참가 물질

5

반응물 3

HCID 180AcetoneHCID 1118Sulfuric AcidHCID 798771,1,3,3-Tetramethylbutyl hydroperoxide

생성물 1

HCID 201968922,2-Di-(t-Octylperoxy) Propane수율 47.8%

시약·촉매·용매 1

HCID 8003Pentane용매

반응 조건

온도
0 °C

실험 절차

To a jacketed reactor was charged 7.0g. (0.12 mole) of acetone, 39.2g. (0.24 mole) of 1,1,3,3-tetramethylbutyl hydroperoxide (89.7% assay) and 120 ml. of pentane. To the vigorously stirred solution at 0°C was added 16g. of 77% sulfuric acid over a period of 30 minutes and the reaction mixture was allowed to stir at 0°C for 4 hours. The pentane layer was then separated, washed with water, then aqueous 10% KOH solution and finally with water to neutral and was dried over anhyd. MgSO4. After separation of the desiccant and vacuum stripping, 21.3g. (53.1% of theory, uncorr.) of liquid remained which had an "active oxygen" content of 8.66% (theory, 9.64%). Hence, the assay was 90% and the corrected yield was 47.8%. An infrared spectrum of the product showed no O--H or C=O bands but showed a strong OO band at 860 cm-1.

후처리

  1. additionTo a jacketed reactor was charged 7.0g
  2. customThe pentane layer was then separated
  3. washwashed with water
  4. dry with materialaqueous 10% KOH solution and finally with water to neutral and was dried over anhyd
  5. customAfter separation of the desiccant and vacuum stripping, 21.3g

출처 및 근거

ORD 기록
ord-c0211e4f19ee41d59a436bc231c8a2a3
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03950432

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