ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Triethylamine → 3-(3,4-Dichlorophenyl)-3-butenol t-butyldimethylsilyl ether

HRID 1279340
ノート
印刷プレビュー

反応式

HRID 1279340 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:9]=[C:10]([C:15](=[CH2:21])[CH2:16][C:17]([O:19]C)=O)[CH:11]=[CH:12][C:13]=1[Cl:14].[OH-].[Na+].C(N(CC)CC)C.[Si:31](Cl)([C:34]([CH3:37])([CH3:36])[CH3:35])([CH3:33])[CH3:32]>O1CCCC1.CN(C)C1C=CN=CC=1.C(OCC)(=O)C.CCCCCC.O>[Si:31]([O:19][CH2:17][CH2:16][C:15]([C:10]1[CH:11]=[CH:12][C:13]([Cl:14])=[C:8]([Cl:7])[CH:9]=1)=[CH2:21])([C:34]([CH3:37])([CH3:36])[CH3:35])([CH3:33])[CH3:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 28928tert-Butyldimethylsilyl chlorideHCID 18427462Methyl 3-(3,4-dichlorophenyl)-3-butenoateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 108712633-(3,4-Dichlorophenyl)-3-butenol t-butyldimethylsilyl ether収率 47%

試薬・触媒・溶媒 5

HCID 142844-(Dimethylamino)pyridine触媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

11.76 g (0.28 mole) of lithium aluminum hydride were suspended in 500 ml of anhydrous tetrahydrofuran, and a solution of 69.06 g (0.28 mole) of methyl 3-(3,4-dichlorophenyl)-3-butenoate [prepared as described in step (a) above] in 500 ml of anhydrous tetrahydrofuran was slowly added dropwise under a nitrogen atmosphere at 0° C. over a period of 15 minutes. The reaction mixture was then stirred at the same temperature for 30 minutes, after which 500 ml of water and 500 ml of a 10% w/v aqueous solution of sodium hydroxide were slowly added. The mixture was then stirred at room temperature for 1 hour. It was then filtered through a Celite (trade mark) filter aid, and the filtrate was extracted three times, each time with 500 ml of ethyl acetate. The combined organic extracts were then dried over anhydrous magnesium sulfate. The solvent was removed from the extract by distillation under reduced pressure, and the resulting residue was dried under reduced pressure. The residue was then dissolved in 250 ml of anhydrous dimethylformamide, and then 47.12 ml (0.34 mole) of triethylamine, 6.88 g (0.06 mole) of 4-dimethylaminopyridine and 50.96 g (0.34 mole) of t-butyldimethylsilyl chloride were added, in that order, whilst ice-cooling. The mixture was then stirred, whilst ice-cooling, for 2 hours. At the end of this time, 1 liter of ethyl acetate was added to the reaction mixture, and the mixture was washed, in turn, with ice-cooled 10% w/v aqueous hydrochloric acid and with a saturated aqueous solution of sodium chloride. It was then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and the resulting residue was purified by silica gel flash column chromatography, using a gradient elution method, with mixtures of hexane and ethyl acetate ranging from 50:1 to 20:1 by volume as the eluent, to obtain 43.52 g (yield 47%) of the title compound as a colorless oil.

後処理

  1. stirringThe mixture was then stirred at room temperature for 1 hour
  2. filtrationIt was then filtered through a Celite (trade mark)
  3. filtrationfilter aid
  4. extractionthe filtrate was extracted three times
  5. dry with materialThe combined organic extracts were then dried over anhydrous magnesium sulfate
  6. customThe solvent was removed from the
  7. extractionextract by distillation under reduced pressure
  8. customthe resulting residue was dried under reduced pressure
  9. dissolutionThe residue was then dissolved in 250 ml of anhydrous dimethylformamide
  10. temperaturecooling
  11. stirringThe mixture was then stirred, whilst ice-
  12. temperaturecooling, for 2 hours
  13. washthe mixture was washed, in turn, with ice-
  14. temperaturecooled 10%
  15. dry with materialIt was then dried over anhydrous magnesium sulfate
  16. customThe solvent was removed by distillation under reduced pressure
  17. customthe resulting residue was purified by silica gel flash column chromatography
  18. washa gradient elution method

出典と根拠

ORDレコード
ord-0eb03229a0e749e19577a050ee107a45
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06448247B1

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート