HRID370459

反应详情

EQUATION

反应方程式

HRID 370459 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

43.5 g of 4-nitrophenoxyacetone crystals were dissolved in 300 ml of ethanol, added portionwise with small amount of sodium boron hydride up to 4.1 g with stirring at room temperature, and stirred thereafter at room temperature for 2 hr. After adding 10 ml of saturated aqueous solution of ammonium chloride under an ice-cold condition in order to decompose the residual sodium borohydride, extraction was carried out with ethyl acetate. The ethyl acetate layer was washed consecutively with water, 3% hydrochloric acid, 5% aqueous solution of sodium hydrogen carbonate, water and saturated saline and subsequently dried with anhydrous sodium sulfate. The solvent was concentrated under reduced pressure and yielded 46.3 g of 2-(4-nitrophenoxy)-1-methylethanol.

WORKUP

后处理

  1. stirringstirred
  2. extractionthe residual sodium borohydride, extraction
  3. washThe ethyl acetate layer was washed consecutively with water, 3% hydrochloric acid, 5% aqueous solution of sodium hydrogen carbonate, water and saturated saline
  4. dry with materialsubsequently dried with anhydrous sodium sulfate
  5. concentrationThe solvent was concentrated under reduced pressure