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Ethylamine → N-ethyl-4-fluorobenzamide

HRID 69590
ノート
印刷プレビュー

反応式

HRID 69590 の反応式
[CH2:1]([NH2:3])[CH3:2].C(N(CC)CC)C.[F:11][C:12]1[CH:20]=[CH:19][C:15]([C:16](Cl)=[O:17])=[CH:14][CH:13]=1>C(Cl)Cl.O>[CH2:1]([NH:3][C:16](=[O:17])[C:15]1[CH:19]=[CH:20][C:12]([F:11])=[CH:13][CH:14]=1)[CH3:2]
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

6

反応物 3

HCID 6341EthylamineHCID 8471TriethylamineHCID 678794-Fluorobenzoyl chloride

生成物 1

HCID 4693101N-ethyl-4-fluorobenzamide収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a solution of ethylamine (69.4 mL, 139 mmol) and triethylamine (21.10 mL, 151 mmol) in DCM (Volume: 150 mL) was added p-Fluorobenzoyl chloride (15.13 mL, 126 mmol) at 0° C. The reaction was stirred at 0° C. for 1 hr and then warmed slowly to room temperature. The reaction mixture was diluted with water. The layers were separated and the organic layer was washed with brine, dried over MgSO4, filtered, and the organic phase stripped to dryness via rotary evaporation. The organic extract was dried in vacuo to provide N-ethyl-4-fluorobenzamide (21 g, 100% yield) as a tan solid.

後処理

  1. temperaturewarmed slowly to room temperature
  2. customThe layers were separated
  3. washthe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe organic phase stripped to dryness via rotary evaporation
  7. extractionThe organic extract
  8. customwas dried in vacuo

出典と根拠

ORDレコード
ord-c44bb80b96884f6e8d8006369addfabe
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822470B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート