HRID863642
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 solution of 30.8 g. ρ-toluoyl chloride and 26.6 g. (0.2 mole) of aluminum chloride in 250 ml. of 1,2-dichloroethane is added to a refluxing solution of 50.6 g. (0.2 mole) of ethyl 3-ethoxycarbonyl-1,4-dimethylpyrrole-2-acetate in 250 ml. of 1,2-dichloroethane over 30 min. The mixture is heated under reflux for 90 min. and poured into ice-dilute hydrochloric acid. The organic solution is separated, washed with brine, and dried over magnesium sulfate. The solven is evaporated in vacuo, and the residue is recrystallized from methanol to give ethyl 1,4-dimethyl-3-ethoxycarbonyl-5-(ρ-toluoyl)-pyrrole-2-acetate as a white solid, M.P. 108°-111° C.
WORKUP
后处理
- temperatureThe mixture is heated
- temperatureunder reflux for 90 min.
- additionpoured into ice-dilute hydrochloric acid
- customThe organic solution is separated
- washwashed with brine
- dry with materialdried over magnesium sulfate
- customThe solven is evaporated in vacuo
- customthe residue is recrystallized from methanol