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Hydrochloric Acid → 2-(3-Oxo-cyclohexyl)-malonic acid dibenzyl ester

HRID 352213
ノート
印刷プレビュー

反応式

HRID 352213 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[Na].[C:8]([O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:13])[CH2:9][C:10]([O-:12])=[O:11].[H-].[Na+].[C:24]1(=[O:30])[CH2:29][CH2:28][CH2:27][CH:26]=[CH:25]1.Cl>C1COCC1>[CH2:15]([O:14][C:8](=[O:13])[CH:9]([CH:26]1[CH2:27][CH2:28][CH2:29][C:24](=[O:30])[CH2:25]1)[C:10]([O:12][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:11])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 135942-Cyclohexen-1-oneHCID 24758Sodium hydrideHCID 5360545SodiumHCID 21226445Aluminium lithium hydrideHCID 22247814Benzyl malonate

生成物 1

HCID 66361702-(3-Oxo-cyclohexyl)-malonic acid dibenzyl ester
収率 141.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a solution of LiAlH4 (6 mL, 6 mmol) under N2 at 0° C. was added a solution of (S)-1,1′-binaphthol (3.43 g, 12 mmol) in THF (48 mL) and stirred for 30 min. The reaction was warmed to RT. To this was added a solution of sodium salt benzyl malonate in THF which was prepared by reacting benzyl malonate (14.99 mL, 60 mmol), NaH (60% by wt., 0.216 g, 5.4 mmol), and THF (60 mL) until all bubbling ceased. Next, cyclohexenone (5.82 mL, 60 mmol) and dibenzlmalonate (1.35 mL, 5.4 mmol) were added and the reaction mixture was stirred overnight. 1.0 N HCl was added and extracted with EtOAc (3×). The combined EtOAc layers were washed (brine), dried (MgSO4), filtered, and concentrated. Flash chromatography (silica gel, acetone/hexanes gradient) gave the title compound (16.17 g, 71%). Mass Spectrum (FIA) (m/z) 381.3 [M+1].

後処理

  1. customwas prepared
  2. stirringthe reaction mixture was stirred overnight
  3. extractionextracted with EtOAc (3×)
  4. washThe combined EtOAc layers were washed (brine)
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-f2db9d22d5154db5a0d3ad6dc5f475cf
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06743794B2

反応ノート

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