反応 #302898

反応方程式

methyl 2-fluoro-3-methylthio-4-(trifluoromethyl)benzoate

sodium methoxide

→

methyl 2-methoxy-3-methylthio-4-(trifluoromethyl)benzoate

収率 18.3%

溶媒

methanol

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度under reflux for 6 h
3. 3
   濃縮For work-up, the mixture was concentrated on a rotary evaporator
4. 4
   抽出the mixture was extracted with dichloromethane
5. 5
   その他The organic phase was dried
6. 6
   抽出extracted with ethyl acetate
7. 7
   その他The organic phase was dried

実験手順

A mixture of 19.9 g (74.2 mmol) of methyl 2-fluoro-3-methylthio-4-(trifluoromethyl)benzoate and 40.1 g (30% by weight, 223 mmol) of sodium methoxide in 250 ml of methanol was heated under reflux for 6 h. For work-up, the mixture was concentrated on a rotary evaporator, the residue was taken up in water and the mixture was extracted with dichloromethane. The organic phase was dried and the filtrate was freed from the solvent. This gave 15.9 g of methyl 2-methoxy-3-methylthio-4-(trifluoromethyl)benzoate as residue. The aqueous phase from the extractive work-up was acidified with dilute hydrochloric acid and extracted with ethyl acetate. The organic phase was dried and the filtrate was freed from the solvent. This gave an additional 3.80 g of methyl 2-methoxy-3-methylthio-4-(trifluoromethyl)benzoate as residue.

出典