Water → 4-(2,2,2-Trimethylacetamido)pyridine

HRID 229037

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HRID 229037 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[C:15](Cl)(=[O:20])[C:16]([CH3:19])([CH3:18])[CH3:17].O>ClCCl>[CH3:17][C:16]([CH3:19])([CH3:18])[C:15]([NH:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1)=[O:20]

참가 물질

6

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온도
0 °C

실험 절차

4-Aminopyridine (4.70 g) and triethylamine (6.31 g) were dissolved in dichloromethane (75 ml) to prepare a solution which was then cooled to 0° C. A solution of pivaloyl chloride (6.63 g) in dichloromethane (10 ml) was gradually added dropwise thereto, and the mixture was stirred at 0° C. for 15 min. Thereafter, the reaction solution was stirred at room temperature overnight. The reaction solution was poured into water (50 ml). The dichloromethane layer was washed with a dilute aqueous sodium hydrogencarbonate solution and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using chloroform to give 2,2-dimethyl-N-pyridin-4-yl-propionamide (7.70 g, yield 87%).

후처리

  1. customto prepare a solution which
  2. stirringThereafter, the reaction solution was stirred at room temperature overnight
  3. washThe dichloromethane layer was washed with a dilute aqueous sodium hydrogencarbonate solution
  4. dry with materialwas dried over anhydrous sodium sulfate
  5. customThe solvent was removed by distillation under the reduced pressure
  6. customthe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-33d579f4efb9499e88804f033d85b257
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560558B2

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