HRID2308379

反应详情

EQUATION

反应方程式

HRID 2308379 的结构方程式

PROCEDURE

实验过程

20 g of anthraquinone was heated at boiling point with 200 ml formamide for 4 hours. The supernatent anthraquinone slowly disappeared while yellow crystals deposited. The solution was cooled, suction filtered and washed thoroughly with alcohol. The resultant 9,10-diformylaminoanthracene was recrystalized from formamide giving long yellow crystals mpt 439° C. Chemical analysis for C16 H12 O2 N2 was calculated N 10.60%, found N10.88%. 40 g of KOH was dissolved in 100 ml of methanol and 10 g of the 9,10 diformylaminoanthracene prepared above was added and formed a deep red brown solution. This was heated at boiling point for one hour, when red glistening crystals separated. The solution was cooled, suction filtered with the exclusion of air and the crystals washed with methanol. The crystal mass was dissolved in acetone, filtered as necessary and the filtrate carefully mixed with petroleum ether to deposit 9,10 diaminoanthracene as glistening flakes. Recrystalization from acetone gave deep red crystals. Chemical analysis for C14 H12 N2 was calculated C 80.75%, H 5.81%, N 13.44% found C 81.06%, H 5.18%, N 12.47%.

WORKUP

后处理

  1. customfor 4 hours
  2. temperatureThe solution was cooled
  3. filtrationsuction filtered
  4. washwashed thoroughly with alcohol
  5. customThe resultant 9,10-diformylaminoanthracene was recrystalized from formamide giving long yellow crystals mpt 439° C
  6. dissolution40 g of KOH was dissolved in 100 ml of methanol
  7. custom10 g of the 9,10 diformylaminoanthracene prepared
  8. additionabove was added
  9. customformed a deep red brown solution
  10. temperatureThis was heated
  11. customfor one hour
  12. customseparated
  13. temperatureThe solution was cooled
  14. filtrationsuction filtered with the exclusion of air
  15. washthe crystals washed with methanol
  16. dissolutionThe crystal mass was dissolved in acetone
  17. filtrationfiltered as necessary and the filtrate
  18. additioncarefully mixed with petroleum ether
  19. customRecrystalization from acetone
  20. customgave deep red crystals