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Triacetoxyperiodinane → 1,1-Dimethylethyl 4-Ethenyl-4-(phenylmethoxymethyl)-1-piperidinecarboxylate

HRID 2213030
ノート
印刷プレビュー

反応式

HRID 2213030 の反応式
[CH3:1]C(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C1=CC=CC=2)=O.O[CH2:24][C:25]1([CH2:38][O:39][CH2:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[CH2:30][CH2:29][N:28]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:27][CH2:26]1.S(=O)(O)[O-].[Na+].C(=O)([O-])O.[Na+]>ClCCl>[CH:24]([C:25]1([CH2:38][O:39][CH2:40][C:41]2[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=2)[CH2:30][CH2:29][N:28]([C:31]([O:33][C:34]([CH3:36])([CH3:35])[CH3:37])=[O:32])[CH2:27][CH2:26]1)=[CH2:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 159087TriacetoxyperiodinaneHCID 516892Sodium BicarbonateHCID 219551981-Boc-4-(hydroxymethyl)-4-[(benzyloxy)methyl]piperidineHCID 23665763Sodium Bisulfite

生成物 1

HCID 219553091,1-Dimethylethyl 4-Ethenyl-4-(phenylmethoxymethyl)-1-piperidinecarboxylate収率 101.6%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

1,1,1-Tris(acetyloxy)-1,1-dihydro-1,2-benziodoxol-3(1H)-one (1.38 g, 3.3 mmol) was added to a solution of 1,1-dimethylethyl 4-(hydroxymethyl)-4-(phenylmethoxymethyl)-1-piperidinecarboxylate (Description 95, 1.06 g, 3 mmol) in dichloromethane (40 mL) and the mixture was stirred at room temperature for 4 hours. Aqueous sodium bisulfite (10%, 10 mL) was added and the mixture was stirred at room temperature for 5 minutes. Saturated aqueous sodium hydrogen carbonate (20 mL) was added and the layers were separated. The organic layer was dried (MgSO4) and the solvent was evaporated under reduced pressure. The residue was dissolved in tetrahydrofuran (20 mL), and added to a stirred, cooled (0° C.) solution of triphenylphosphoranylidine (0.1M, 50 mL). The mixture was stirred at room temperature for 16 hours, then the solvent was evaporated under reduced pressure. Ethyl acetate (40 mL) and aqueous sodium hydrogen carbonate (10%, 40 mL) were added and the layers were separated. The organic layer was dried (MgSO4) and the solvent was evaporated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with isohexane/EtOAc (75:25) give the title compound (1.01 g, 99%). m/z (ES+) 332 (M+1).

後処理

  1. stirringthe mixture was stirred at room temperature for 5 minutes
  2. customthe layers were separated
  3. dry with materialThe organic layer was dried (MgSO4)
  4. customthe solvent was evaporated under reduced pressure
  5. dissolutionThe residue was dissolved in tetrahydrofuran (20 mL)
  6. additionadded to a stirred
  7. temperaturecooled (0° C.) solution of triphenylphosphoranylidine (0.1M, 50 mL)
  8. stirringThe mixture was stirred at room temperature for 16 hours
  9. customthe solvent was evaporated under reduced pressure
  10. additionEthyl acetate (40 mL) and aqueous sodium hydrogen carbonate (10%, 40 mL) were added
  11. customthe layers were separated
  12. dry with materialThe organic layer was dried (MgSO4)
  13. customthe solvent was evaporated under reduced pressure
  14. customThe residue was purified by flash column chromatography on silica gel
  15. washeluting with isohexane/EtOAc (75:25)

出典と根拠

ORDレコード
ord-faf33270296f4658b32b656d9e75887d
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07105507B2

反応ノート

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