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Tetrahydrofuran → 1-Bromo-4-(ethenyloxy)benzene

HRID 1099545
ノート
印刷プレビュー

反応式

HRID 1099545 の反応式
C(O[K])(C)(C)C.O1CCCC1.[Br:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:20][CH2:21]Cl)=[CH:15][CH:14]=1>O>[Br:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH:20]=[CH2:21])=[CH:15][CH:14]=1
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 8028Tetrahydrofuran2 回HCID 1086801-Bromo-4-(2-chloroethoxy)benzeneHCID 178418922HCID 178418922、化合物

生成物 1

HCID 114013721-Bromo-4-(ethenyloxy)benzene収率 79%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Tert-Butoxypotassium (33.7 g, 300 mmol) was added to a solution of tetrahydrofuran (hereinafter THF) (250 mL) containing 1-bromo-4-(2-chloroethoxy)benzene (58.6 g, 249 mmol) prepared in Example 6 (6a) over 10 minutes at −10° C. The mixture was stirred at room temperature for 21 hours, and water (500 mL) was added thereto. The resulting mixture was extracted with methyl tert-butyl ether (200 mL, 150 mL) twice. The organic layers were combined, washed with saturated brine (100 mL) twice, and dried over anhydrous magnesium sulfate. Then, the solvent was evaporated. The resulting residue was dissolved in hexane (100 mL), and the precipitated insoluble substance was removed by filtration. The insoluble substance was further washed with hexane (5 mL) five times. The filtrates were combined, concentrated, and purified by silica gel column chromatography (hexane) to give 39.0 g of the title compound (colorless oil, yield: 79%).

後処理

  1. extractionThe resulting mixture was extracted with methyl tert-butyl ether (200 mL, 150 mL) twice
  2. washwashed with saturated brine (100 mL) twice
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThen, the solvent was evaporated
  5. dissolutionThe resulting residue was dissolved in hexane (100 mL)
  6. customthe precipitated insoluble substance was removed by filtration
  7. washThe insoluble substance was further washed with hexane (5 mL) five times
  8. concentrationconcentrated
  9. custompurified by silica gel column chromatography (hexane)

出典と根拠

ORDレコード
ord-b57b3620b4bc4eabac9813b1a060ce8d
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08143446B2

反応ノート

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