HRID1943626

反应详情

EQUATION

反应方程式

HRID 1943626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1H-pyrido[2,3-b][1,4]oxazin-2-one (113 mg, 0.75 mmol) was dissolved in tetrahydrofuran (3.5 ml) and then cooled to 0□. 1.0M Lithium aluminum hydride dissolved in tetrahydrofuran (1.5 ml, 1.5 mmol) was added thereto dropwise. After stirring for 2 hours at room temperature, 0.1 ml of water, 0.2 ml of 10% aqueous solution of sodium hydroxide, and 0.3 ml of water were added in this order under stirring. After filtering precipitates, the filtrate was extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure to obtain colorless liquid (90 mg, 88%).

WORKUP

后处理

  1. temperaturecooled to 0□
  2. additionwas added
  3. stirringunder stirring
  4. filtrationAfter filtering
  5. customprecipitates
  6. extractionthe filtrate was extracted with ethyl acetate
  7. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate (Na2SO4)
  8. filtrationfiltered
  9. customevaporated under reduced pressure