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1,1-Dibromoethane → HCID 178492974, 화합물

HRID 2186527
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HRID 2186527 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

HCID 178492974HCID 178492974, 화합물

시약·촉매·용매 2

HCID 193501Copper;dilithium;tetrachloride촉매
HCID 8028
Tetrahydrofuran
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-912c8d44997d4e46b16e06fbb582f44f
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06403814B1

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