反应 #302898

反应方程式

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

sodium methoxide

→

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

收率 18.3%

溶剂

methanol

反应条件

后处理

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

实验过程

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.

来源