1-Acetylnaphthalene → 2-Bromo-1-(1-naphthalenyl)ethanone

HRID 386394

反応式

HRID 386394 の反応式
[C:1]1([C:11](=[O:13])[CH3:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[Br:14]Br>O1CCOCC1>[Br:14][CH2:12][C:11]([C:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1)=[O:13]

参加物

4

反応物 2

HCID 136631-AcetylnaphthaleneHCID 24408Bromine

生成物 1

HCID 38305132-Bromo-1-(1-naphthalenyl)ethanone収率 93.2%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of 1-(naphthalen-1-yl)ethanone (500 mg, 2.9 mmol) in dioxane (5 mL) was added to a solution of bromine (510 mg, 3.19 mmol) in dioxane (10 mL), at room temperature, over a period of 30 minutes. The reaction mixture was then stirred at room temperature for 20 minutes and concentrated. The resulting residue was diluted with ether and washed with saturated sodium bicarbonate, water, dried over sodium sulfate and concentrated. Purification by preparative thin layer chromatography (70% DCM/30% hexanes) afforded 2-bromo-1-(naphthalen-1-yl)ethanone (673 mg, 93%).

後処理

  1. concentrationconcentrated
  2. additionThe resulting residue was diluted with ether
  3. washwashed with saturated sodium bicarbonate, water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customPurification by preparative thin layer chromatography (70% DCM/30% hexanes)

出典と根拠

ORDレコード
ord-28433479610f4dd89803e5dd0db30856
出典データセット
uspto-grants-2013_02
特許番号
US08372807B2

関連ノート

読み込み中…