HRID1608470

反应详情

EQUATION

反应方程式

HRID 1608470 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A heterogeneous mixture of 71.7 g of 1,5-bis-(4'-methoxycarbonyl-phenyl)-1,4-pentadien-3-one, 3.8 grams of 5% Pd on carbon, and 650 mL of 2-propanol was prepared in a 1 L 3-necked flask. The mixture was stirred mechanically and heated to 50° C. The system was flushed with hydrogen, and hydrogen was then supplied on a continuous basis at about 20 psi. The hydrogen uptake was initially very rapid, but gradually slowed. When hydrogen uptake nearly ceased, the hydrogen source was removed. The vessel was heated to 75°-80° C. and purged thoroughly with nitrogen. The hot product was filtered through a steam-jacketed Buchner funnel which contained a pad of filter-aid. The hot filtrate immediately began to precipitate the product.

WORKUP

后处理

  1. customwas prepared in a 1 L 3-necked flask
  2. customThe system was flushed with hydrogen, and hydrogen
  3. customthe hydrogen source was removed
  4. temperatureThe vessel was heated to 75°-80° C.
  5. custompurged thoroughly with nitrogen
  6. filtrationThe hot product was filtered through a steam-jacketed Buchner funnel which
  7. filtrationof filter-aid
  8. customto precipitate the product