反应详情

0.636 g of sodium borohydride was added to 22 mL of ice-cooled ethanol, to which a solution of 1.09 g of calcium chloride in 14 mL of ethanol was added dropwise, followed by addition of 1.20 g of 5-(ethoxycarbonyl)-2-pyridinecarboxylic acid ½ calcium salt, and this mixture was stirred for one hour at room temperature. The reaction mixture, to which 2.8 mL of concentrated sulfuric acid was added, was stirred for 6 hours while heating it under reflux. The reaction mixture was cooled to room temperature and concentrated under reduced pressure followed by successive addition of a saturated aqueous solution of sodium hydrogen carbonate and chloroform, and then the organic phase was separated therefrom. The resultant organic phase was washed with a saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was distilled out under reduced pressure to yield 0.34 g of ethyl 5-(hydroxymethyl)-2-pyridinecarboxylate as light yellow solid.

1. stirringwas stirred for 6 hours
2. temperaturewhile heating it
3. temperatureunder reflux
4. temperatureThe reaction mixture was cooled to room temperature
5. concentrationconcentrated under reduced pressure
6. additionfollowed by successive addition of a saturated aqueous solution of sodium hydrogen carbonate and chloroform
7. customthe organic phase was separated
8. washThe resultant organic phase was washed with a saturated sodium chloride solution
9. dry with materialdried over anhydrous magnesium sulfate
10. distillationthe solvent was distilled out under reduced pressure