HRID379082
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
Sodium carbonate (13.8 g) is added to a solution of 1,2-dichloro-3-nitrobenzene (19.29 g) and 2,4-dichlorothio-phenol (17.9 g) in xylene (250 ml), and the resulting mixture is heated for 5 hours at reflux temperature. The precipitate is separated by filtration, washed with xylene and the combined organic phases are concentrated. The resultant residue is mixed with petroleum ether and stirred for 1 hour at room temperature. Following this, the crystalline material is suction filtered and washed with petroleum ether, and any remaining solvent is removed in a vacuum. Yield: 25.6 g of colourless crystals (76.6%).
WORKUP
后处理
- temperaturethe resulting mixture is heated for 5 hours
- temperatureat reflux temperature
- customThe precipitate is separated by filtration
- washwashed with xylene
- concentrationthe combined organic phases are concentrated
- additionThe resultant residue is mixed with petroleum ether
- filtrationfiltered
- washwashed with petroleum ether
- customany remaining solvent is removed in a vacuum