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Triethylsilane → 3-Bromo-(5-ethyl-2-thienylmethyl)benzene

HRID 1514508
ノート
印刷プレビュー

反応式

HRID 1514508 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]([C:10]2[S:11][C:12]([CH2:15][CH3:16])=[CH:13][CH:14]=2)O)[CH:5]=[CH:6][CH:7]=1.C([SiH](CC)CC)C.C(=O)([O-])O.[Na+]>ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][C:10]2[S:11][C:12]([CH2:15][CH3:16])=[CH:13][CH:14]=2)[CH:5]=[CH:6][CH:7]=1
参加物反応条件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 12052TriethylsilaneHCID 516892Sodium BicarbonateHCID 611008623-Bromophenyl-5-ethyl-2-thienylmethanol

生成物 1

HCID 469304303-Bromo-(5-ethyl-2-thienylmethyl)benzene収率 93.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-78 °C

実験手順

A solution of 1,3-dibromobenzene (3.7 g) in tetrahydrofuran (25 ml) was cooled to −78° C. under argon atmosphere, and thereto was added dropwise n-butyl lithium (2.44 M hexane solution, 5.55 ml). The reaction mixture was stirred at the same temperature for 10 minutes, and thereto was added dropwise a solution of 5-ethyl-2-thiophenecarboxaldehyde (2.0 g) in tetrahydrofuran (10 ml). The mixture was stirred at the same temperature for 30 minutes, and thereto was added a saturated ammonium chloride solution, and the reaction mixture was warmed to room temperature. The mixture was extracted with ethyl acetate, and the extract was dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=97:3-85:15) to give 3-bromophenyl-5-ethyl-2-thienylmethanol (2.97 g) as a pale yellow syrup. APCI-Mass m/Z 279/281 (M+H—H2O). (2) The above 3-bromophenyl-5-ethyl-2-thienylmethanol (2.90 g) was dissolved in dichloromethane (38 ml), and the mixture was cooled to −78° C. under argon atmosphere. To the mixture were added triethylsilane (6.18 ml) and boron trifluoride•diethyl ether complex (2.45 ml), and the mixture was gradually warmed to room temperature over a period of one hour. The mixture was basified with a saturated aqueous sodium hydrogen carbonate solution, and the dichloromethane layer was collected, dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane) to give the desired 3-bromo-(5-ethyl-2-thienylmethyl)benzene (2.57 g) as a colorless syrup. APCI-Mass m/Z 281/283 (M+H).

後処理

  1. temperaturethe mixture was gradually warmed to room temperature over a period of one hour
  2. customthe dichloromethane layer was collected
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane)

出典と根拠

ORDレコード
ord-bb0a7283412449b58691b9bff8b61f97
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08222219B2

反応ノート

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