Ethyl Acetate → 8-Methylidene-1,4-dioxaspiro[4.5]decane

HRID 1966812노트

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HRID 1966812 반응식
[CH3:1]C(C)([O-])C.[K+].CI.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[O:28]1[C:32]2([CH2:37][CH2:36][C:35](=O)[CH2:34][CH2:33]2)[O:31][CH2:30][CH2:29]1.C(OCC)(=O)C>O1CCCC1.O>[CH2:1]=[C:35]1[CH2:36][CH2:37][C:32]2([O:31][CH2:30][CH2:29][O:28]2)[CH2:33][CH2:34]1

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 5674151,4-Dioxaspiro[4.5]decan-8-oneHCID 13401130HCID 13401130, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 109537438-Methylidene-1,4-dioxaspiro[4.5]decane

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

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온도
-78 °C

실험 절차

Potassium tert-butoxide (3.230 gm, 28.812 mmol) and triphenylphosphine methyl iodide (10.286 gm, 28.812 mmol) were dissolved in dry tetrahydrofuran (30 ml). The mixture was cooled to −78° C. and stirred at the same temperature for about 15 minutes. 1,4-Dioxaspiro[4.5]decan-8-one (3.0 gm, 19.208 mmol) in tetrahydrofuran was added drop wise and the mixture was stirred at the same temperature for about 30 minutes and then it was warmed to room temperature and stirred overnight, extaction was done with ethyl acetate and water. The organic layer was dried over sodium sulphate and concentrated. Purification was done by column chromatography.

후처리

  1. stirringthe mixture was stirred at the same temperature for about 30 minutes
  2. temperatureit was warmed to room temperature
  3. stirringstirred overnight
  4. dry with materialThe organic layer was dried over sodium sulphate
  5. concentrationconcentrated
  6. customPurification

출처 및 근거

ORD 기록
ord-a70918488f4a43a5a602075749591145
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08420666B2

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