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Sodium Methoxide → HCID 20339555, 화합물

HRID 1395537
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HRID 1395537 반응식
[CH3:1][N:2]([CH3:13])[CH2:3][CH2:4][NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8](Cl)[N:7]=1.[CH3:14][O-:15].[Na+]>CN(C)C=O>[CH3:1][N:2]([CH3:13])[CH2:3][CH2:4][NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:15][CH3:14])[N:7]=1
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참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 20339561N1-(6-Chloropyridin-2-yl)-N2,N2-dimethylethane-1,2-diamine

생성물 1

HCID 20339555HCID 20339555, 화합물수율 80.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 2-(2-dimethylaminoethylamino)-6-chloropyridine (10.0 g, 0.05 mole) in dimethylformamide (50 ml) containing sodium methoxide (3.5 gm, 0.065 mole) is heated at 110°-120° for two hours. The solution is cooled and the sodium chloride filtered. After removing the solvent in vacuo, the residue is dissolved in dilute hydrochloric acid (10%), washed with methylene chloride, made alkaline with sodium carbonate and the product is extracted into methylene chloride. After drying this solution over anhydrous sodium sulfate and filtering through charcoal, the solvent is removed under vacuum to give the oily product (7.9 g). This is used without further purification in the succeeding step.

후처리

  1. temperatureis heated at 110°-120° for two hours
  2. temperatureThe solution is cooled
  3. filtrationthe sodium chloride filtered
  4. customAfter removing the solvent in vacuo
  5. dissolutionthe residue is dissolved in dilute hydrochloric acid (10%)
  6. washwashed with methylene chloride
  7. extractionthe product is extracted into methylene chloride
  8. dry with materialAfter drying this solution over anhydrous sodium sulfate
  9. filtrationfiltering through charcoal
  10. customthe solvent is removed under vacuum

출처 및 근거

ORD 기록
ord-21dd9ff70d834e4cb6a093ee6610dbf6
출처 데이터셋
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04203988

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