反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a solution of 2-methylcyclohexyl 2-chloro-5-(benzoylamino)benzoate (1.8 g, 0.0048 mole) in toluene (100 ml) was added Lawesson's Reagent (2.5 g), sodium bicarbonate (1.0 g) to produce the reaction mixture. The reaction mixture was stirred and refluxed for 4 hours. The reaction mixture was then cooled to ambient temperature which resulted in the formation of a white solid precipitate. The white solid was filtered off. The filtrate was then passed through a short column of aluminum oxide (neutral) using ether/hexane as eluent to give a yellow solution. The yellow solution was concentrated and a yellow solid crystallized. The yellow solid was filtered to give 2-methylcyclohexyl 2-chloro-5[(phenylthiomethyl)amino]benzoate as a yellow solid (1.3 g, m.p. 143°-144° C.).
WORKUP
后处理
- customto produce the reaction mixture
- temperaturerefluxed for 4 hours
- customresulted in the formation of a white solid precipitate
- filtrationThe white solid was filtered off
- customto give a yellow solution
- concentrationThe yellow solution was concentrated
- customa yellow solid crystallized
- filtrationThe yellow solid was filtered