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1,1-Dibromoethane → HCID 178492974、化合物

HRID 2186527
ノート
印刷プレビュー

反応式

HRID 2186527 の反応式
[Mg:1].BrC(Br)C.[CH3:6][O:7][C:8]1[CH:13]=[CH:12][C:11](Br)=[C:10]([O:15][CH3:16])[C:9]=1[O:17][CH3:18].[Br-:19].C1COCC1>C1COCC1.[Li+].[Li+].[Cl-].[Cl-].[Cl-].[Cl-].[Cu+2]>[CH3:6][O:7][C:8]1[CH:13]=[C:12]([Mg:1][Br:19])[CH:11]=[C:10]([O:15][CH3:16])[C:9]=1[O:17][CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 112011,1-DibromoethaneHCID 2569301-Bromo-2,3,4-trimethoxybenzeneHCID 5462224MagnesiumHCID 86744366Bromide tetrahydrofuran

生成物 1

HCID 178492974HCID 178492974、化合物

試薬・触媒・溶媒 2

HCID 193501Copper;dilithium;tetrachloride触媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

Magnesium (0.82 g, 33.74 mmol) was taken in flame dried 100 ml two necked flask and dry TEF (20 ml) was added. Then the dibromo ethane (0.1 ml) and trimethoxy bromobenzene (0.3 g, 1.20 mmol) were added at room temperature and stirred for 20 mins. The reaction initiates as indicated by temperature rise. The remaining bromide/THF (8.8 g, 35.48 mmol) in THF (20 ml) was added over 15 mints. After the addition was completed reaction mixture was stirred at 25° C. under nitrogen for 18 h. To the Grignard reagent at 0° C. was added a solution of dilithium tetrachlorocuprate (0.5 M, 0.76 ml, 0.38 mmol). The reaction was stirred at 0° C. for 15 mints and was used immediately for the coupling reaction.

後処理

  1. temperaturein flame
  2. dry with materialdried 100 ml two necked flask
  3. customdry TEF (20 ml)
  4. additionwas added
  5. additionAfter the addition
  6. customreaction mixture
  7. stirringwas stirred at 25° C. under nitrogen for 18 h
  8. stirringThe reaction was stirred at 0° C. for 15 mints
  9. customwas used immediately for the coupling reaction

出典と根拠

ORDレコード
ord-912c8d44997d4e46b16e06fbb582f44f
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06403814B1

反応ノート

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