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Mesityl oxide → HCID 20570470, 화합물

HRID 1577965
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HRID 1577965 반응식
[O:1]=[C:2]([CH:4]=[C:5]([CH3:7])[CH3:6])[CH3:3].[C:8]([O:12][O:13][C:14]([CH3:23])([CH3:22])[CH2:15][CH2:16][C:17]([O:20][OH:21])([CH3:19])[CH3:18])([CH3:11])([CH3:10])[CH3:9]>>[CH3:6][C:5]([O:21][O:20][C:17]([CH3:19])([CH3:18])[CH2:16][CH2:15][C:14]([O:13][O:12][C:8]([CH3:11])([CH3:10])[CH3:9])([CH3:23])[CH3:22])([CH2:4][C:2](=[O:1])[CH3:3])[CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 8858Mesityl oxideHCID 1410462,5-Dimethyl-2-hydroperoxide-5-tert-butylperoxyhexane

생성물 1

HCID 20570470HCID 20570470, 화합물수율 84.4%

실험 절차

A mixture of 19.62 g. (0.20 mole) of mesityl oxide, 61.40 g. (0.22 mole) of 4-t-butylperoxy-1,1,4,4-tetramethylbutyl hydroperoxide (84%) and 10.0 g. of Amberlyst 15® sulfonic acid type ion exchange resin was stirred for 16 hours at 28°-30° C. and then at 35° C. for 4 hours. The resin was separated by filtration and the filtrate subjected to steam distillation at 20 torr in the presence of sodium bicarbonate to maintain a slightly alkaline pH during the distillation. The distillation was ended when the removal of unreacted mesityl oxide was complete. The product was taken up in ether, the ether solution dried over anhydrous magnesium sulfate and the ether removed under reduced pressure. The product weighed 55.9 g. and was obtained in 84.4% yield.

후처리

  1. addition
A mixture of 19.62 g
  • customThe resin was separated by filtration
  • distillationthe filtrate subjected to steam distillation at 20 torr in the presence of sodium bicarbonate
  • temperatureto maintain a slightly alkaline pH
  • distillationduring the distillation
  • distillationThe distillation
  • customthe removal of unreacted mesityl oxide
  • dry with materialthe ether solution dried over anhydrous magnesium sulfate
  • customthe ether removed under reduced pressure
  • customand was obtained in 84.4% yield
  • 출처 및 근거

    ORD 기록
    ord-3eb57120c65343c684ca9f074e534b52
    출처 데이터셋
    uspto-grants-1981_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04289914

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