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
Into a 1000 ml round-bottomed flask equipped with a stirrer, thermometer and Marcusson-condenser 180 g (3 moles) of n-propanol, and 380 g of benzene are weighed in, whereupon 493 g (2 moles) of 4-chloro-3,5-dinitro-benzoic acid and 20 g of concentrated sulfuric acid are added under stirring. The reaction mixture is heated to boiling on a water bath under stirring (86° C.) until no more water is distilled off. The water thus formed is collected in the Marcusson-condenser and removed if necessary. In the meantime the upper benzene/n-propanol phase is continuously re-introduced into the flask. The reaction having been completed the mixture is cooled to room temperature under stirring, the precipitated crystals are filtered off, washed with cold n-propanol and dried. Thus 490 g of the desired compound are obtained, yield 85%, purity 98%.
WORKUP
后处理
- customInto a 1000 ml round-bottomed flask equipped with a stirrer
- temperatureThe reaction mixture is heated
- customto boiling on a water bath
- distillationis distilled off
- customThe water thus formed
- customis collected in the Marcusson-condenser
- customremoved if necessary
- additionIn the meantime the upper benzene/n-propanol phase is continuously re-introduced into the flask
- stirringunder stirring
- filtrationthe precipitated crystals are filtered off
- washwashed with cold n-propanol
- customdried