反应详情

4-Chlorobenzotrifluoride (31.36 ml, 235.26 mmol) was dissolved in anhydrous DMF (200 ml), and mercaptoethanol (15.00 ml, 213.87 mmol) and K2CO3 (38.43 g, 278.06 mmol) were added thereto. The mixture was stirred for 30 minutes at room temperature and then refluxed. After 15 hours have passed, the reaction mixture was cooled to room temperature and the reaction was stopped by adding distilled water. The reaction mixture was extracted with diethyl ether, and the organic layer was washed with aqueous NH4Cl solution, dried over anhydrous MgSO4, and concentrated. The reaction solution thus concentrated was purified by silica gel column chromatography (EA/n-hexane=1/3, v/v) to give 2-(4-trifluoromethyl-phenylsulfanyl)-ethanol (32.11 g, 67.56%) of a colorless oil.

1. temperaturerefluxed
2. waitAfter 15 hours have passed
3. temperaturethe reaction mixture was cooled to room temperature
4. additionby adding
5. distillationdistilled water
6. extractionThe reaction mixture was extracted with diethyl ether
7. washthe organic layer was washed with aqueous NH4Cl solution
8. dry with materialdried over anhydrous MgSO4
9. concentrationconcentrated
10. concentrationThe reaction solution thus concentrated
11. customwas purified by silica gel column chromatography (EA/n-hexane=1/3