HRID979990

反应详情

EQUATION

反应方程式

HRID 979990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a pressure reactor were placed 1.5 g (4.57 m mole) of methyl 6-chloro-3-methylflavone-8-carboxylate, 1.8 g (14.2 m mole) of sodium acetate, 150 ml of isopropanol and 0.075 g of 5% palladium-carbon. After the atmosphere was replaced with hydrogen gas, reaction was conducted at 70° C. under a pressure of 5.0 kg/cm2G for 6 hours. Thereafter the contents were withdrawn from the reactor and were subjected to filtration while being hot to remove the catalyst. The solvent was recovered from the filtrate to provide 1.1 g (82.1%) of white needle-like crystals which melt at 162.2° to 164.8° C. The crystals were recrystallized from alcohol to obtain a product having a melting point of 166.4° to 168.2° C. The product was found identical in melting point with the compound prepared by the conventional method. When the product of this example and the compound prepared by the conventional method were melted together, the melting point was not lower than that of the product of this example.

WORKUP

后处理

  1. customInto a pressure reactor were placed
  2. customThereafter the contents were withdrawn from the reactor
  3. filtrationwere subjected to filtration
  4. customto remove the catalyst
  5. customThe solvent was recovered from the filtrate