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

HRID 1295081
ノート
印刷プレビュー

反応式

HRID 1295081 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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 determined 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).

後処理

  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)

出典と根拠

ORDレコード
ord-1b2e43b1957b479e9c1acbacfbbef675
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07241792B2

反応ノート

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