HRID874958

反应详情

EQUATION

反应方程式

HRID 874958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

8-Hydroxyquinoline (14 mg) was added to a solution of 6-(4-(4-cyanobutanoyl)-3-methylpiperazin-1-yl)nicotinonitrile (0.9 g, 3.03 mmol) in ethanol (25 mL). Hydroxylamine hydrochloride (440 mg, 6.36 mmol) in water (4 mL), followed by sodium carbonate (510 mg, 4.81 mmol) in water (3 mL), were added to this solution and the reaction mixture was heated to reflux for 3 h. Ethanol was then removed under reduced pressure, and the product was extracted with EtOAc. The combined extracts were dried over anhydrous sodium sulfate, and concentrated under reduced pressure to afford 5-(4-(5-cyanopyridin-2-yl)-2-methylpiperazin-1-yl)-N′-hydroxy-5-oxopentanimidamide (400 mg, crude), which was carried through without further purification. MS (ESI) m/z: Calculated for C16H22N6O2: 330.18. found: 331.1 (M+H)+

WORKUP

后处理

  1. additionwere added to this solution
  2. temperaturethe reaction mixture was heated
  3. temperatureto reflux for 3 h
  4. customEthanol was then removed under reduced pressure
  5. extractionthe product was extracted with EtOAc
  6. dry with materialThe combined extracts were dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure