反応 #45283

反応方程式

NaH

trifluoromethanesulfonyl chloride

2,2,2-trifluoro-1-(4-fluoro-phenyl)ethanol

→

trifluoromethanesulfonic acid 2,2,2-trifluoro-1-(4-fluorophenyl)ethyl ester

収率 101.2%

溶媒

hexane

diethyl ether

diethyl ether

diethyl ether

反応条件

後処理

1. 1
   workup.WAITAfter 2 h
2. 2
   その他the reaction mixture was quenched
3. 3
   workup.ADDITIONby adding a solution of NaHCO3
4. 4
   抽出the product was extracted with diethyl ether
5. 5
   洗浄The extracts were washed with brine
6. 6
   その他dried
7. 7
   その他the solvent was removed

実験手順

NaH (640 mg, 16 mmol, 60% in mineral oil) was washed twice with hexane (20 mL) and then suspended in dried diethyl ether (20 mL). A solution of 2,2,2-trifluoro-1-(4-fluoro-phenyl)ethanol (1.94 g, 10 mmol) in diethyl ether (10 mL) was added at 0° C. After stirring for 2 h at room temperature, a solution of trifluoromethanesulfonyl chloride (1.68 g, 10 mmol) in diethyl ether (10 mL) was added. After 2 h, the reaction mixture was quenched by adding a solution of NaHCO3 and the product was extracted with diethyl ether. The extracts were washed with brine and dried, and the solvent was removed to yield trifluoromethanesulfonic acid 2,2,2-trifluoro-1-(4-fluorophenyl)ethyl ester (3.3 g).

出典