HRID2261353

反应详情

EQUATION

反应方程式

HRID 2261353 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9.91 g of {[5-(1-hydroxy-1-methylethyl)-isoxazol-3-yl]methylidene}malononitrile was dissolved in 100 ml of tetrahydrofuran, and 3.78 g of sodium borohydride was then added under ice-cooling. The mixture was stirred for 8 hours under ice-cooling. The reaction mixture was added to 0.5 N hydrochloric acid over 30 minutes and then extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 5.38 g of {[5-(1-hydroxy-1-methylethyl)-isoxazol-3-yl]methyl}malononitrile.

WORKUP

后处理

  1. temperaturecooling
  2. temperaturecooling
  3. extractionextracted with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure