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Sodium hydride → (R,Z)-2-(hex-3-enyl)oxirane

HRID 1432815
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HRID 1432815 반응식
[CH2:1]([OH:10])[C@H:2](O)[CH2:3][CH2:4]/[CH:5]=[CH:6]\[CH2:7][CH3:8].[H-].[Na+].C(C1C=CC(S(Cl)(=O)=O)=C(C(C)C)C=1C(C)C)(C)C>C1COCC1>[CH2:3]([C@@H:2]1[CH2:1][O:10]1)[CH2:4]/[CH:5]=[CH:6]\[CH2:7][CH3:8]
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참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 11514985Triisopropylbenzenesulfonyl chlorideHCID 58906721(R,Z)-oct-5-ene-1,2-diol

생성물 1

HCID 58906753(R,Z)-2-(hex-3-enyl)oxirane

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (R,Z)-oct-5-ene-1,2-diol (8.50 g, 58.9 mmol) in THF (230 mL) at 0° C. was added NaH (60% dispersion in mineral oil, 7.06 g, 177 mmol) (7.06 g as dispersion). The mixture was warmed to ambient temperature and stirred for 40 min. The reaction was cooled to 0° C. and triisopropylbenzenesulfonyl chloride (20.7 g, 61.8 mmol) was added. The reaction was warmed to room temp, stirred for 1 h, quenched with H2O and extracted with Et2O. The organics were washed with brine, dried over MgSO4, filtered, and concentrated. Purification by silica gel chromatography (2% Et2O in pentane gradient to 8% Et2O in pentane) gave (R,Z)-2-(hex-3-enyl)oxirane. It was determiined that slight racemization occurred at this step (98% ee to 84% ee). In order to ensure optical purity the enantioenriched product was further resolved using Jacobsen's hydrolytic kinetic resolution (HKR, Step E). 1H NMR (400 MHz, CDCl3): δ 5.41 (1H, m), 5.35 (1H, m), 2.93 (1H, m), 2.75 (1H, dd, J=5.2, 4.4 Hz), 2.49 (1H, dd, J=5.2, 2.8 Hz), 2.20 (2H, q, J=6.8 Hz), 2.06 (2H, quin, 7.6 Hz); 1.59 (2H, m), 0.97 (3H, t, J=7.6 Hz).

후처리

  1. temperatureThe reaction was cooled to 0° C.
  2. temperatureThe reaction was warmed to room temp
  3. stirringstirred for 1 h
  4. customquenched with H2O
  5. extractionextracted with Et2O
  6. washThe organics were washed with brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customPurification by silica gel chromatography (2% Et2O in pentane gradient to 8% Et2O in pentane)

출처 및 근거

ORD 기록
ord-caf523f482c54e79af7094c5e60aef4e
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612106B2

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