HRID887729

反应详情

EQUATION

反应方程式

HRID 887729 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

3-Amino-4-bromo-6-chloro-pyridine-2-carboxylic acid methyl ester (169 mg) was suspended in methanol (3 mL) and 2N sodium hydroxide solution (2 mL). The suspension was stirred at 50° C. for 3 hours. The precipitate was filtered off and washed carefully with diethyl ether. The precipitate was dissolved in a mixture of 2N hydrochloric acid and ethyl acetate and the layers were separated. The aqueous layer was 2× extracted with ethyl acetate, washed with brine, dried over MgSO4 and concentrated in vacuum to afford 138 mg of the title compound of the formula

WORKUP

后处理

  1. filtrationThe precipitate was filtered off
  2. washwashed carefully with diethyl ether
  3. dissolutionThe precipitate was dissolved in a mixture of 2N hydrochloric acid and ethyl acetate
  4. customthe layers were separated
  5. extractionextracted with ethyl acetate
  6. washwashed with brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuum