HRID1720874

反应详情

EQUATION

反应方程式

HRID 1720874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,6-dichloro-3-nitrobenzoic acid (4.72 g, 0.02 mol), 4-tertbutylaniline (4.47 g, 0.03 mol), lithium carbonate (1.48 g, 0.02 mol), and 1-propanol (10 mL) was refluxed with stirring for 20 h. The solvent was evaporated and to the residue, water (30 mL) and benzene (50 mL) were added. The mixture was made strongly basic with sodium hydroxide and stirred for 1h. Orange precipitate was collected by filtration and washed with benzene and ether. Dry precipitate was dissolved in water and acidified with diluted hydrochloric acid. Resulting precipitate was collected and crystallized from acetone-water to give 4.55 (65%) of the desired product, mp 201°-204° C. Anal. (C31H27N7O6) C, H, N.

WORKUP

后处理

  1. temperaturewas refluxed
  2. customThe solvent was evaporated and to the residue, water (30 mL) and benzene (50 mL)
  3. additionwere added
  4. stirringstirred for 1h
  5. filtrationOrange precipitate was collected by filtration
  6. washwashed with benzene and ether
  7. customDry precipitate
  8. dissolutionwas dissolved in water
  9. customResulting precipitate
  10. customwas collected
  11. customcrystallized from acetone-water