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m-Chloroperbenzoic acid → HCID 15332454, 화합물

HRID 487517
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HRID 487517 반응식
ClC1C=C(C=CC=1)C(OO)=[O:6].[CH3:12][C:13]([CH2:15][CH:16]([CH3:23])[CH2:17][CH:18]([CH3:22])[CH2:19][CH2:20][CH3:21])=[CH2:14]>C(Cl)Cl>[CH3:14][C:13]1([CH2:15][CH:16]([CH3:23])[CH2:17][CH:18]([CH3:22])[CH2:19][CH2:20][CH3:21])[O:6][CH2:12]1
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 5361182,4,6-Trimethyl-1-nonene

생성물 1

HCID 15332454HCID 15332454, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
10 °C

실험 절차

m-Chloroperoxybenzoic acid (7.31 g, 60% purity, 25.42 mmol) was added to a stirred solution of 2,4,6-trimethyl-1-nonene (5) (3.56 g, 21.19 mmol) in 70 ml of dry methylene chloride in a 250 ml flask in an ice bath. The chilled reaction mixture was stirred for one hour, and then stirred vigorously overnight at room temperature. The reaction mixture was cooled to 10° C. before filtering out a white slurry, which was washed with cooled methylene chloride. The combined filtrates were washed three times with cooled aqueous carbonate, water, and brine and dried over sodium sulfate. Evaporation of the solvent yielded a crude oil which was distilled at 65°-70° C. and 1.5 mm Hg to yield pure 2,4,6-trimethyl-1,2-epoxynonane (6).

후처리

  1. customThe chilled reaction mixture
  2. stirringstirred vigorously overnight at room temperature
  3. filtrationbefore filtering out a white slurry, which
  4. washwas washed with cooled methylene chloride
  5. washThe combined filtrates were washed three times with cooled aqueous carbonate, water, and brine
  6. dry with materialdried over sodium sulfate
  7. customEvaporation of the solvent
  8. customyielded a crude oil which
  9. distillationwas distilled at 65°-70° C.

출처 및 근거

ORD 기록
ord-9371c626af0e4c8299d2837964360e61
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05296220

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