反応 #1880953

反応方程式

4-hydroxy-2-trifluoromethylthiophene

2,6-difluoropyridine

DMF

K2CO3

→

2-fluoro-6-(2-trifluoromethyl-4-thienyloxy)pyridine

収率 74.3%

溶媒

water

反応条件

後処理

1. 1
   温度cooled to RT
2. 2
   抽出After extraction twice with heptane/ethyl acetate (1:1)
3. 3
   洗浄twice with ethyl acetate the product is washed with water and saturated sodium chloride solution
4. 4
   乾燥dried over MgSO4
5. 5
   濃縮concentrated
6. 6
   その他Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent

実験手順

1.00 g of 2,6-difluoropyridine is introduced into 10 ml of DMF under nitrogen and 1.44 g of K2CO3 are added at RT. 1.61 g of 4-hydroxy-2-trifluoromethylthiophene are added and the mixture is heated at 80° C. for 4 h, then cooled to RT and poured into water. After extraction twice with heptane/ethyl acetate (1:1) and twice with ethyl acetate the product is washed with water and saturated sodium chloride solution, dried over MgSO4 and concentrated. Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent gives 1.7 g of 2-fluoro-6-(2-trifluoromethyl-4-thienyloxy)pyridine as a colorless oil.

出典