HRID1770243

反应详情

EQUATION

反应方程式

HRID 1770243 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

The previously prepared butoxypropionitrile (224.8 grams) was combined with Raney nickel (20 grams of 50/50 mixture with water) in a 1-liter stainless steel autoclave along with a premixed ethanol/ammonium hydroxide solution (37.5 grams of ammonium hydroxide and 212.5 grams of ethanol). The addition of the ammonium hydroxide limits the reaction that leads to the formation of by-product dibutoxypropylamine. After purging with nitrogen, the reactor was pressurized with 500 psi of hydrogen and heated to 60° C. After 20 hours at this temperature, the reactor was cooled to room temperature and the product discharged. The product was filtered to remove the Raney nickel and then distilled using a simple Vigreux column to extract the butoxypropylamine. The distillation produced a yield of about 79.5% of product and 18.3% of the secondary amine.

WORKUP

后处理

  1. customthe reaction that
  2. customAfter purging with nitrogen
  3. temperaturethe reactor was cooled to room temperature
  4. filtrationThe product was filtered
  5. customto remove the Raney nickel
  6. distillationdistilled
  7. extractionto extract the butoxypropylamine
  8. distillationThe distillation