HRID893497

反应详情

EQUATION

反应方程式

HRID 893497 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A solution of 0.13 g of (±)-cis-4-(cyanomethyl)-1,5-dioxaspiro[5.5]undecane-2-acetic acid in 20 mL of methanol saturated with anhydrous ammonia is added to a Parr shaker bottle containing 0.2 g of water wet Raney nickel #30. The solution is heated at 40° C. and 50 pounds per square inch gage (psig) hydrogen pressure for 17 hours. The suspension is cooled and filtered to remove the Raney nickel through filter aid and the precipitate is washed with methanol. The filtrate is concentrated at reduced pressure The residue is dissolved in methanol saturated with anhydrous ammonia, treated with decolorizing charcoal, filtered through filter aid and evaporated to give 0.13 g of (±)-cis-4-(2-aminoethyl)-1,5-dioxaspiro-[5.5]undecane-2-acetic acid.

WORKUP

后处理

  1. temperatureThe suspension is cooled
  2. filtrationfiltered
  3. customto remove the Raney nickel
  4. filtrationthrough filter aid
  5. washthe precipitate is washed with methanol
  6. concentrationThe filtrate is concentrated at reduced pressure The residue
  7. dissolutionis dissolved in methanol saturated with anhydrous ammonia
  8. additiontreated with decolorizing charcoal
  9. filtrationfiltered
  10. filtrationthrough filter aid
  11. customevaporated