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1,2-Dibromoethane → Methyl 1-(3-methylisoxazol-5-yl)cyclopropanecarboxylate

HRID 931069
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HRID 931069 반응식
[CH3:1][C:2]1[CH:6]=[C:5]([CH2:7][C:8]([O:10][CH3:11])=[O:9])[O:4][N:3]=1.[H-].[Na+].Br[CH2:15][CH2:16]Br.C(=O)(O)[O-].[Na+]>CN(C)C=O>[CH3:1][C:2]1[CH:6]=[C:5]([C:7]2([C:8]([O:10][CH3:11])=[O:9])[CH2:16][CH2:15]2)[O:4][N:3]=1
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참가 물질

6

반응물 4

HCID 78391,2-DibromoethaneHCID 24758Sodium hydrideHCID 516892Sodium BicarbonateHCID 12366875Methyl 2-(3-methylisoxazol-5-yl)acetate

생성물 1

HCID 89853625Methyl 1-(3-methylisoxazol-5-yl)cyclopropanecarboxylate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Into a 15 mL round bottom flask was added methyl 2-(3-methylisoxazol-5-yl)acetate (250 mg, 1.61 mmol) dissolved in N,N-dimethylformamide (7 mL) followed by addition of sodium hydride (60% suspension in mineral oil, 322 mg, 8.06 mmol). The mixture was stirred at room temperature for 15 minutes. 1,2-Dibromoethane (417 μL, 4.83 mmol) was added dropwise. The reaction mixture was stirred at room temperature for 18 h. A saturated aqueous solution of sodium bicarbonate was added to the mixture and it was extracted with dichloromethane (3×). The combined organics were washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was dissolved in dichloromethane (1.5 mL) and washed (3×) with an aqueous (10%) lithium chloride solution to remove residues of N,N-dimethylformamide. The organics were dried over sodium sulfate, decanted and concentrated under reduced pressure to afford methyl 1-(3-methylisoxazol-5-yl)cyclopropanecarboxylate MS (ES+) (M+H) 182.0; LCMS retention time: 2.53 minutes (Method L). The material was used for the next step without further purification.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 18 h
  2. extractionwas extracted with dichloromethane (3×)
  3. washThe combined organics were washed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. dissolutionThe residue was dissolved in dichloromethane (1.5 mL)
  8. washwashed (3×) with an aqueous (10%) lithium chloride solution
  9. customto remove residues of N,N-dimethylformamide
  10. dry with materialThe organics were dried over sodium sulfate
  11. customdecanted
  12. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ed29fe56eda4482289792036b2f06559
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296745B2

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