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
Methyl p-tolyl sulfide (75 g, 542.27 mmol) was diluted in chorobenzene (452 mL). N-Chloro Succinimide (NCS) (76.07 g, 1.05 eq) was added in small portions maintaining the temperature between 35° C. and 45° C., under an argon atmosphere. The reaction mixture was stirred at the same temperature range until the reaction was complete. After that time, the solution turned into a suspension. The suspension formed was filtered and the solid was washed with chlorobenzene (50 ml). The filtrate was washed with water (3×225 mL). The resulting organic phase was dried with magnesium sulfate and concentrated. The crude product was purified by distillation to give 102.68 g (100%) of the desired product as yellow oil (bp: 96° C. at 40 Pa).
WORKUP
后处理
- temperaturemaintaining the temperature between 35° C. and 45° C.
- customThe suspension formed
- filtrationwas filtered
- washthe solid was washed with chlorobenzene (50 ml)
- washThe filtrate was washed with water (3×225 mL)
- dry with materialThe resulting organic phase was dried with magnesium sulfate
- concentrationconcentrated
- distillationThe crude product was purified by distillation