反応 #4849

反応方程式

methanol

2-methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzenepropanoic acid

sulfuric acid

→

methyl 2-methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzenepropanoate

溶媒

toluene

反応条件

後処理

1. 1
   温度heated
2. 2
   温度at reflux for 18 hours
3. 3
   濃縮concentrated to 20 ml at reduced pressure
4. 4
   抽出extracted with ether
5. 5
   洗浄The resulting ether solution is washed with 5% sodium bicarbonate solution and water
6. 6
   乾燥The solution is dried with anhydrous magnesium sulfate
7. 7
   ろ過filtered
8. 8
   濃縮concentrated at reduced pressure
9. 9
   その他to obtain a residual solid which
10. 10
    その他is recrystallized from petroleum ether

実験手順

To a solution of 50 ml of methanol in 50 ml toluene are added 7.0 g (0.02 mole) of 2-methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzenepropanoic acid and 1 ml of concentrated sulfuric acid. The resulting solution is stirred, heated at reflux for 18 hours, then concentrated to 20 ml at reduced pressure, and extracted with ether. The resulting ether solution is washed with 5% sodium bicarbonate solution and water. The solution is dried with anhydrous magnesium sulfate, filtered and concentrated at reduced pressure to obtain a residual solid which is recrystallized from petroleum ether to give 5.5 g of methyl 2-methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzenepropanoate having a melting point of 78°-80°.

出典