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Water → HCID 87088126, 화합물

HRID 1053542
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HRID 1053542 반응식
[CH2:1]([OH:21])[CH2:2][CH2:3][CH2:4]/[CH:5]=[CH:6]\[CH2:7]/[CH:8]=[CH:9]\[CH2:10]/[CH:11]=[CH:12]\[CH2:13]/[CH:14]=[CH:15]\[CH2:16]/[CH:17]=[CH:18]\[CH2:19][CH3:20].[C:22]([O:26]Br)(=[O:25])[CH2:23][CH3:24].[OH-].[Na+].O.[C:31]1([CH3:37])[CH:36]=CC=C[CH:32]=1>[Cl-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH2:1]([O:21][CH:23]([CH3:24])[C:22]([O:26][C:31]([CH3:37])([CH3:36])[CH3:32])=[O:25])[CH2:2][CH2:3][CH2:4]/[CH:5]=[CH:6]\[CH2:7]/[CH:8]=[CH:9]\[CH2:10]/[CH:11]=[CH:12]\[CH2:13]/[CH:14]=[CH:15]\[CH2:16]/[CH:17]=[CH:18]\[CH2:19][CH3:20]
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참가 물질

7

반응물 5

HCID 962WaterHCID 1140TolueneHCID 14798Sodium HydroxideHCID 11228909Hypobromous acid, anhydride with propanoic acidHCID 59539494(5Z,8Z,11Z,14Z,17Z)-icosa-5,8,11,14,17-pentaen-1-ol

생성물 1

HCID 87088126HCID 87088126, 화합물수율 90%

시약·촉매·용매 1

HCID 70681Tetrabutylammonium Chloride촉매

실험 절차

A mixture of (5Z,8Z,11Z,14Z,17Z)-icosa-5,8,11,14,17-pentaen-1-ol, (1.00 g, 3.47 mmol), tetrabutylammonium chloride (0.24 g, 0.87 mmol) and t-butyl □-bromo propionate (3.62 g, 17.3 mmol) was dissolved in toluene (36 mL) and placed under nitrogen. An aqueous solution of sodium hydroxide (50%, 8 mL) was added slowly under vigorous stirring and the resulting mixture was stirred at ambient temperature for twenty hours. Water was added and the mixture was extracted three times with ether. The combined organic extract was washed with brine, dried (Na2SO4), filtered and concentrated. The residue was purified by flash chromatography on silica gel using 2% ethyl acetate in heptane as eluent. Concentration of the appropriate fractions afforded 1.40 g (90% yield) of the title compound as an oil. 1H-NMR (300 MHz, CDCl3): δ 0.95 (t, 3H), 1.41 (d, 3H), 1.48 (s, 9H), 1.48-1.66 (m, 4H), 2.05 (m, 4H), 2.83 (m, 8H), 3.35 (m, 1H), 3.55 (m, 1H), 3.79 (q, 1H), 5.32-5.44 (m, 10H).

후처리

  1. stirringthe resulting mixture was stirred at ambient temperature for twenty hours
  2. extractionthe mixture was extracted three times with ether
  3. extractionThe combined organic extract
  4. washwas washed with brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified by flash chromatography on silica gel using 2% ethyl acetate in heptane as eluent

출처 및 근거

ORD 기록
ord-07caf6a8b2a14f6481c3773f66f89098
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394228B2

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