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Water → HCID 178447997、化合物

HRID 1377121
ノート
印刷プレビュー

反応式

HRID 1377121 の反応式
[F:1]/[C:2](/[C@H:9]1[CH2:14][CH2:13][C@H:12]([CH2:15][CH2:16][CH3:17])[CH2:11][CH2:10]1)=[C:3](/[F:8])\[Si](C)(C)C.[F-].[K+].O>C(#N)C>[F:1]/[C:2](/[C@H:9]1[CH2:14][CH2:13][C@H:12]([CH2:15][CH2:16][CH3:17])[CH2:11][CH2:10]1)=[CH:3]/[F:8]
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 962Water2 回HCID 522689Potassium FluorideHCID 178448000HCID 178448000、化合物

生成物 1

HCID 178447997HCID 178447997、化合物収率 80%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Then, 18.2 g (0.07 mol) of the obtained (Z)-1,2-difluoro-1-(trans-4-n-propylcyclohexyl)-2-trimethylsilylethylene was dissolved in 50 ml of acetonitrile, and then 8.12 g (0.14 mol) of potassium fluoride and 3.78 g (0.21 mol) of water were added thereto. The mixture was reacted for one hour at 50° C. The reaction mixture was cooled, and then 200 ml of water was added thereto. The mixture was extracted with methylene chloride. The organic layer was washed with a saturated sodium chloride aqueous solution and dried over CaCl2. After filtration, the solvent and low boiling substances were distilled off, and the residue was further distilled under reduced pressure to obtain 10.5 g (yield: 80%) of (E)-1,2-difluoro-1-(trans-4-n-propylcyclohexyl)ethylene.

後処理

  1. customThe mixture was reacted for one hour at 50° C
  2. temperatureThe reaction mixture was cooled
  3. extractionThe mixture was extracted with methylene chloride
  4. washThe organic layer was washed with a saturated sodium chloride aqueous solution
  5. dry with materialdried over CaCl2
  6. filtrationAfter filtration
  7. distillationthe solvent and low boiling substances were distilled off
  8. distillationthe residue was further distilled under reduced pressure

出典と根拠

ORDレコード
ord-237d0beadd6941d2af0a3b054dacff5b
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05663463

反応ノート

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