反応 #450269

反応方程式

3-ethyl-4-[3-(4-trifluoromethoxyphenoxy)propyloxy]-5-methylphenol

potassium carbonate

1,1,3-trichloro-1-propene

→

3-ethyl-4-[3-(4-trifluoromethoxyphenoxy)propyloxy]-5-methyl-1-(3,3-dichloro-2-propenyloxy)benzene

収率 71.0%

溶媒

N,N-dimethylformamide

N,N-dimethylformamide

反応条件

後処理

1. 1
   workup.STIRRINGAfter stirring at room temperature for 12 hours
2. 2
   抽出extracted twice with 100 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 0.6 g of 3-ethyl-4-[3-(4-trifluoromethoxyphenoxy)propyloxy]-5-methylphenol, 0.22 g of potassium carbonate and 10 ml of N,N-dimethylformamide was added dropwise a solution of 0.31 g of 1,1,3-trichloro-1-propene dissolved in 5 ml of N,N-dimethylformamide, while stirring at room temperature. After stirring at room temperature for 12 hours, the reaction mixture was poured into ice-water, and extracted twice with 100 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 0.5 g of 3-ethyl-4-[3-(4-trifluoromethoxyphenoxy)propyloxy]-5-methyl-1-(3,3-dichloro-2-propenyloxy)benzene (71% yield), nD23.5 1.5150.

出典