反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed
- customThe solvent was evaporated and to the residue, water (30 mL) and benzene (50 mL)
- additionwere added
- stirringstirred for 1h
- filtrationOrange precipitate was collected by filtration
- washwashed with benzene and ether
- customDry precipitate
- dissolutionwas dissolved in water
- customResulting precipitate
- customwas collected
- customcrystallized from acetone-water