HRID565019
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
In 20 ml of pyridine was dissolved 1.2 g (5.52 mmol) of ethyl 4-amino-1-methyl-2-indolecarboxylate. While stirring at room temperature, 10 ml of anhydrous acetic acid was added to the solution. After stirring for 2 hours at room temperature, the reaction mixture was poured onto ice water. The mixture was extracted three times with ethyl acetate. The combined extracts were washed with 1N hydrochloric acid and then with saturated sodium hydrogencarbonate solution. The solvent was then distilled off under reduced pressure and the residue was purified by silica gel column chromatography to give 1.40 g (97.9%) of ethyl 4-acetamido-1-methyl-2-indolecarboxylate.
WORKUP
后处理
- stirringAfter stirring for 2 hours at room temperature
- additionthe reaction mixture was poured onto ice water
- extractionThe mixture was extracted three times with ethyl acetate
- washThe combined extracts were washed with 1N hydrochloric acid
- distillationThe solvent was then distilled off under reduced pressure
- customthe residue was purified by silica gel column chromatography