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

5-Hexenal → 1,1,1-Trifluoro-6-hepten-2-ol

HRID 520266
ノート
印刷プレビュー

反応式

HRID 520266 の反応式
[CH:1](=[O:7])[CH2:2][CH2:3][CH2:4][CH:5]=[CH2:6].C[Si](C)(C)[C:10]([F:13])([F:12])[F:11]>C1COCC1.F.C([N+](CCCC)(CCCC)CCCC)CCC>[F:11][C:10]([F:13])([F:12])[CH:1]([OH:7])[CH2:2][CH2:3][CH2:4][CH:5]=[CH2:6]
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 2

HCID 698175-HexenalHCID 552549(Trifluoromethyl)trimethylsilane

生成物 1

HCID 541076021,1,1-Trifluoro-6-hepten-2-ol収率 31%

試薬・触媒・溶媒 2

HCID 18424689Tetrabutylammonium hydrofluoride触媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a ice-bath cooled solution of hex-5-enal (500 mg, 4.331 mmol) and trimethyl(trifluoromethyl)silane (0.74 g, 5.13 mmol, 1.2 equiv.) in THF (10 mL) was added tetrabutylammonium hydrofluoride (10 mg, 0.04 mmol). The ice bath was removed and the reaction progress was monitored via GCMS and 1H NMR. Upon complete transformation of the starting material the reaction mixture was treated with 2M HCl and stirred for an additional 2 h. Then, 50 mL of Et2O was introduced and the layers were separated. The aqueous fraction was additionally extracted with Et2O and the combined organic phases were washed sequentially with a saturated aqueous NaHCO3 solution, water, and brine. After drying with MgSO4 and filtration the solvent was removed under reduced pressure and the resultant crude residue was purified by column chromatography (silica gel, pentane/Et2O, v/v=8/2). Fractions containing the pure compound were collected and concentrated in vacuo to give 1,1,1-trifluorohept-6-en-2-ol (225 mg, 31% yield) as a yellow oil.

後処理

  1. customThe ice bath was removed
  2. additionUpon complete transformation of the starting material the reaction mixture was treated with 2M HCl
  3. additionThen, 50 mL of Et2O was introduced
  4. customthe layers were separated
  5. extractionThe aqueous fraction was additionally extracted with Et2O
  6. washthe combined organic phases were washed sequentially with a saturated aqueous NaHCO3 solution, water, and brine
  7. dry with materialAfter drying with MgSO4 and filtration the solvent
  8. customwas removed under reduced pressure
  9. customthe resultant crude residue was purified by column chromatography (silica gel, pentane/Et2O, v/v=8/2)
  10. additionFractions containing the pure compound
  11. customwere collected
  12. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b9cfe71ab0de4373b6ab9dda6a18135a
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09326513B2

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