反应 #586139

反应方程式

[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-nitrophenyl] isopropyl sulfide

compound

methyl 2-propylthio-4-(3-trifluoromethylpyrazolyl)benzoate

water

acetic acid

→

4-(2,6-dichloro-4-trifluoromethylphenyl)-2-isopropylthioaniline

收率 36.0%

溶剂

toluene

toluene

反应条件

后处理

1. 1
   温度with reflux
2. 2
   温度heating for another 3 hours
3. 3
   过滤The insolubles were filtered off
4. 4
   其他the filtrate was separated with water and toluene
5. 5
   洗涤The toluene layer was washed with water
6. 6
   干燥dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
8. 8
   其他Purification of the residue by silica gel column chromatography

实验过程

3.5 g (63.6 mmol) of iron powder, 10 m of water and 1 m of acetic acid were stirred in 20 ml toluene at 60° C. for 30 minutes, and 3.0 g (7.3 mmol) of [5-(2,6-dichloro-4-trifluoromethylphenyl)-2-nitrophenyl] isopropyl sulfide (the compound prepared in Example 8 (2)) in 10 ml toluene was added dropwise. The reaction was carried out with reflux and heating for another 3 hours, and then the reaction mixture was cooled to room temperature. The insolubles were filtered off, and the filtrate was separated with water and toluene. The toluene layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 1.0 g of 4-(2,6-dichloro-4-trifluoromethylphenyl)-2-isopropylthioaniline (yield 36.0%) as a pale yellow dough (nD20 1.5782).

来源