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Isobutyl iodide → [1-(2-Methylpropyl)cyclohexyl]methanol

HRID 1778849
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HRID 1778849 반응식
C([N-]C(C)C)(C)C.[Li+].[CH:9]1([C:15]([O:17]C)=O)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.I[CH2:20][CH:21]([CH3:23])[CH3:22]>O1CCCC1>[CH2:20]([C:9]1([CH2:15][OH:17])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]1)[CH:21]([CH3:23])[CH3:22]
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참가 물질

5

반응물 3

HCID 10556Isobutyl iodideHCID 20748Methyl cyclohexanecarboxylateHCID 2724682Lithium diisopropylamide

생성물 1

HCID 66024992[1-(2-Methylpropyl)cyclohexyl]methanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of lithium diisopropylamide (2.0 M, 7.74 mL) at −78° C. was added methyl cyclohexanecarboxylate (2.0 g) dropwise as a solution in tetrahydrofuran (20 mL). After stirring for 30 minutes. 1-iodo-2-methylpropane (1.956 mL) was added dropwise as a solution in tetrahydrofuran (1 mL). The reaction was allowed to warm to room temperature and stirred overnight. The reaction was quenched with 1N HCl (25 mL) and diluted with water (25 mL) and extracted into diethyl ether (50 mL). The ether layer was washed with brine (30 mL), dried over magnesium sulfate, filtered and concentrated. The residue was dissolved in diethyl ether (25 mL) and lithium aluminum hydride (1.0M in tetrahydrofuran, 16.88 mL) was added dropwise. After stirring overnight, the reaction was quenched with water (0.65 mL), 15% aqueous NaOH (0.65 mL), more water (1.95 mL), then magnesium sulfate was added and the reaction filtered and concentrated. The residue was loaded onto silica gel and eluted using a gradient of 3% to 20% ethyl acetate/hexanes to provide the title compound.

후처리

  1. stirringstirred overnight
  2. customThe reaction was quenched with 1N HCl (25 mL)
  3. additiondiluted with water (25 mL)
  4. extractionextracted into diethyl ether (50 mL)
  5. washThe ether layer was washed with brine (30 mL)
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. dissolutionThe residue was dissolved in diethyl ether (25 mL)
  10. additionlithium aluminum hydride (1.0M in tetrahydrofuran, 16.88 mL) was added dropwise
  11. stirringAfter stirring overnight
  12. customthe reaction was quenched with water (0.65 mL), 15% aqueous NaOH (0.65 mL), more water (1.95 mL)
  13. additionmagnesium sulfate was added
  14. filtrationthe reaction filtered
  15. concentrationconcentrated
  16. washeluted

출처 및 근거

ORD 기록
ord-e189d6a4523e4c429aebdf7f29736d4f
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09266877B2

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