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

HRID 1430240
ノート
印刷プレビュー

反応式

HRID 1430240 の反応式
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]
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 10556Isobutyl iodideHCID 20748Methyl cyclohexanecarboxylateHCID 2724682Lithium diisopropylamide

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9440da4ab2ab4ffbbd0ef81a1443f5d8
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08940737B2

反応ノート

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