反应详情

20 g 2-(2,4-dinitrophenyl)ethanol (94 mmol) are dissolved in 120 ml abs. toluene and 4 ml pyridine. 34 g thidnyl chloride (21 ml, 282 mmol) in 20 ml abs. toluene are quickly added in a drop-wise manner. After 2 h under reflux, this is cooled and poured onto ice. This is mixed with 100 ml CH2Cl2 and the aqueous phase is extracted 2× each with 50 ml CH2Cl2. The combined organic phases are dried over Na2SO4, filtered and rotary evaporated. 21.51 g (93 mmol, 98%) 2-(2,4-dinitrophenyl)ethyl chloride are obtained as a brown oil.

1. temperatureAfter 2 h under reflux
2. temperaturethis is cooled
3. additionpoured onto ice
4. extractionthe aqueous phase is extracted 2× each with 50 ml CH2Cl2
5. dry with materialThe combined organic phases are dried over Na2SO4
6. filtrationfiltered