反応 #450243

反応方程式

3,5-dichloro-4-(1,1,2,2-tetrafluoroethoxy)phenol

potassium carbonate

1,1,3-trichloro-1-propene

→

3,5-dichloro-4-(1,1,2,2-tetrafluoroethoxy)-1-(3,3-dichloro-2-propenyloxy)benzene

収率 82.0%

溶媒

N,N-dimethylformamide

N,N-dimethylformamide

反応条件

後処理

1. 1
   workup.STIRRINGAfter stirring
2. 2
   抽出extracted twice with 40 ml of diethyl ether
3. 3
   洗浄The combined ether layer was washed with water
4. 4
   乾燥dried with anhydrous magnesium sulfate
5. 5
   濃縮concentrated
6. 6
   その他to obtain a crude product

実験手順

To a mixture of 600 mg of 3,5-dichloro-4-(1,1,2,2-tetrafluoroethoxy)phenol, 330 mg of potassium carbonate and 10 ml of N,N-dimethylformamide was added dropwise a solution of 340 mg of 1,1,3-trichloro-1-propene dissolved in 3 ml of N,N-dimethylformamide, while stirring at room temperature. After stirring continued at room temperature for 5 hours, the reaction mixture was poured into ice-water, and extracted twice with 40 ml of diethyl ether. The combined ether layer was washed with water, dried with anhydrous magnesium sulfate, and concentrated to obtain a crude product. The crude product was subjected to silica gel chromatography, which afforded 630 mg of 3,5-dichloro-4-(1,1,2,2-tetrafluoroethoxy)-1-(3,3-dichloro-2-propenyloxy)benzene (82% yield), nD24.6 1.5067.

出典