反応 #2005557

反応方程式

2,2-difluoro-7-hydroxy-benzo[1,3]dioxole-5-carboxylic acid methyl ester

1-(bromo-ethyl)-3-methyl-benzene

K2CO3

DMF

→

title compound

収率 88.4%

2,2-Difluoro-7-(2-m-tolyl-ethoxy)-benzo[1,3]dioxole-5-carboxylic acid methyl ester

収率 88.4%

溶媒

water

反応条件

後処理

1. 1
   温度to cool to room temperature
2. 2
   抽出extracted three times
3. 3
   その他The organic layer was then dried
4. 4
   その他evaporated

実験手順

1.8 g of 2,2-difluoro-7-hydroxy-benzo[1,3]dioxole-5-carboxylic acid methyl ester, 4.6 g of 1-(bromo-ethyl)-3-methyl-benzene, and 3.2 g of K2CO3 were added to 70 ml of anhydrous DMF and the reaction mixture stirred at 80° C. for 3 h. The reaction mixture was then allowed to cool to room temperature, 300 ml of water added and extracted three times using 100 ml of EA each. The organic layer was then dried using MgSO4 and evaporated. Chromatography on silica gel using EA/HEP 1:4 yielded 2.4 g of the title compound, colorless oil. Rf (EA/HEP 1:4)=0.32

出典