HRID570721

反应详情

EQUATION

反应方程式

HRID 570721 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dimethyl 6-aminopyridine-2,5-dicarboxylate (395 mg) was suspended in a mixed solvent (16 ml) of tetrahydrofuran/ethanol (1/1), calcium chloride (834 mg) and sodium borohydride (85.5 mg) were added thereto under ice-cooling, and the mixture was stirred for 2 hr. The reaction mixture was acidified with 1M hydrochloric acid, basified with saturated aqueous potassium carbonate solution, and extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give the title compound (296 mg) as a white solid.

WORKUP

后处理

  1. additionwere added
  2. temperatureunder ice-cooling
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure