Benzoyl Peroxide → Di-n-octylphosphinic acid

HRID 9515

반응식

HRID 9515 반응식
[CH2:1]([PH:9](=[O:11])[OH:10])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH2:12]=[CH:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(O)C>[CH2:1]([P:9]([CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])(=[O:10])[OH:11])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

참가 물질

5

반응물 3

HCID 7187Benzoyl Peroxide3회HCID 81251-OcteneHCID 178418940HCID 178418940, 화합물

생성물 1

HCID 99411Di-n-octylphosphinic acid수율 48.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred mixture of 46.5 g (0.261 mol) of n-octylphosphinic acid in 250 mL 95% ethanol, 1-octene (58.6 g, 0.5218 mol) was added followed by 9.042 g (0.026 mol) of 70% benzoyl peroxide. The resulting mixture was refluxed for 8 hs, and then another 6.758 g (0.0196 mol) of benzoyl peroxide was added and the reaction continued to reflux for an extra 8 hs. A third 4.244 g of benzoyl peroxide was added (0.01305 mol) and refluxing continued for an extra 8 hs. The resulting mixture was cooled in the refrigerator, filtered, and 11.8 g of di-n-octylphosphinic acid was recovered using a rotary evaporator. The solid was washed with 100 mL of cooled 95% ethanol and the filtrate was concentrated on the rotary vacuum and replaced in the refrigerator. Another 24.9 g di-n-octylphosphinic acid was obtained on cooling to attain a total of 36.7 g (48.4% yield).

후처리

  1. additionwas added
  2. temperatureThe resulting mixture was refluxed for 8 hs
  3. temperatureto reflux for an extra 8 hs
  4. temperaturerefluxing
  5. temperatureThe resulting mixture was cooled in the refrigerator
  6. filtrationfiltered
  7. custom11.8 g of di-n-octylphosphinic acid was recovered
  8. customa rotary evaporator
  9. washThe solid was washed with 100 mL of cooled 95% ethanol
  10. concentrationthe filtrate was concentrated on the rotary vacuum

출처 및 근거

ORD 기록
ord-f858daf9b78340f8a6c06509c19a3d65
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091262B2

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