HRID221562

反应详情

EQUATION

反应方程式

HRID 221562 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triethylamine (12.8 mL, 91.8 mmol) was added to a solution of 4-chloro-3-nitroquinoline (8.0 g, 38 mmol) in DMF (100 mL). The resulting solution was stirred for five minutes at room temperature, and then ethyl 3-aminobutyrate (6.2 mL, 42 mmol) was added. The reaction was stirred overnight at room temperature and poured into deionized water (320 mL). The mixture was extracted with ethyl acetate (1×125 mL and 2×100 mL). The combined extracts were washed with brine (3×120 mL), dried over magnesium sulfate, filtered through a layer of CELITE filter agent, concentrated under reduced pressure, and further dried under high vacuum to provide 11.5 g of ethyl 3-[(3-nitroquinolin-4-yl)amino]butanoate as a yellow solid.

WORKUP

后处理

  1. stirringThe reaction was stirred overnight at room temperature
  2. extractionThe mixture was extracted with ethyl acetate (1×125 mL and 2×100 mL)
  3. washThe combined extracts were washed with brine (3×120 mL)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered through a layer of CELITE filter agent
  6. concentrationconcentrated under reduced pressure
  7. customfurther dried under high vacuum