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

HRID 931069
笔记
打印预览

反应方程式

HRID 931069 反应方程式
[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
参与物实验过程后处理来源与证据反应笔记

参与物

6

反应物 4

HCID 78391,2-DibromoethaneHCID 24758氢化钠HCID 516892碳酸氢钠HCID 12366875Methyl 2-(3-methylisoxazol-5-yl)acetate

产物 1

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

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-ed29fe56eda4482289792036b2f06559
来源数据集
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
专利号
US09296745B2

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记