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Dimethylamine → 4-Bromo-2-(dimethylaminomethyl)-1-fluorobenzene

HRID 1066841
ノート
印刷プレビュー

反応式

HRID 1066841 の反応式
[F:1][C:2]1[CH:9]=[CH:8][C:7]([Br:10])=[CH:6][C:3]=1[CH2:4]Br.[CH3:11][NH:12][CH3:13]>CO>[CH3:11][N:12]([CH2:4][C:3]1[CH:6]=[C:7]([Br:10])[CH:8]=[CH:9][C:2]=1[F:1])[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 674DimethylamineHCID 135532954-Bromo-2-(bromomethyl)-1-fluorobenzene

生成物 1

HCID 211961754-Bromo-2-(dimethylaminomethyl)-1-fluorobenzene

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

In a 50 ml flask, under a nitrogen atmosphere, 2-fluoro-5-bromobenzyl bromide (1.264 g, 4.72 mmol) was dissolved in methanol (10 ml). Dimethylamine (8 M in H2O, 1.77 ml, 14.2 mmol) was added as a solution in methanol (5 ml), and the resulting mixture was stirred at ambient temperature for about two hours. The progress of the reaction was monitored by thin layer chromatography. The methanol was removed by evaporation. The residue was partitioned between 1 M potassium carbonate and diethyl ether. The aqueous fraction was back extracted with diethyl ether. The organic fractions were combined, washed with brine (7×) and dried over sodium sulfate. The solvents were removed in vacuo. The title intermediate was used without further purification.

後処理

  1. customThe methanol was removed by evaporation
  2. customThe residue was partitioned between 1 M potassium carbonate and diethyl ether
  3. extractionThe aqueous fraction was back extracted with diethyl ether
  4. washwashed with brine (7×)
  5. dry with materialdried over sodium sulfate
  6. customThe solvents were removed in vacuo
  7. customThe title intermediate was used without further purification

出典と根拠

ORDレコード
ord-8d679847236e4b9daf1a1484f9bdf501
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06245761B1

反応ノート

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