HRID2300930

反应详情

EQUATION

反应方程式

HRID 2300930 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-ethoxycarbonyl-3-nitropyridine (0.5 g, 2.5 mmoL, 1 eq.) in 20 mL of methanol and 5 mL of water was added lithium hydroxide (0.2 g, 4.5 mmoL, 1.8 eq.) and the mixture stirred for 16 hours at ambient temperature. The reaction was concentrated and 50 mL of 1N KOH was were added. The solution was washed with 25 mL of ethyl actetate, acidified with 1 N HCl, and extracted with ethyl acetate (3×50 mL). The combined ethyl acetate extractions were dried over sodium sulfate and concentrated to give 2-carboxy-3-nitropyridine as a yellow solid (0.4 g, 95% yield).

WORKUP

后处理

  1. concentrationThe reaction was concentrated
  2. addition50 mL of 1N KOH was were added
  3. washThe solution was washed with 25 mL of ethyl actetate
  4. extractionextracted with ethyl acetate (3×50 mL)
  5. extractionThe combined ethyl acetate extractions
  6. dry with materialwere dried over sodium sulfate
  7. concentrationconcentrated