反应详情

To a solution prepared by dissolving 0.44 g of 2-trifluoromethyl-4-(3-ethoxyphenoxy)phenol in 10 ml of N,N-dimethylformamide, 0.062 g of sodium hydride (60% oil-based) was added with stirring under ice cooling. After 10 minutes, a solution prepared by dissolving 0.24 g of 1,1,3-trichloro-1-propene in 5 ml of N,N-dimethylformamide was added dropwise under ice cooling. After stirring at room temperature for 10 hours, the reaction solution was poured into ice-water, and extracted twice with 50 ml of diethyl ether. Then, the ether layers were combined, washed with water, dried over anhydrous magnesium sulfate and concentrated to give a crude product. This crude product was subjected to silica gel chromatography to give 0.37 g of 2-trifluoromethyl-4-(3-ethoxyphenoxy)-1-(3,3-dichloro-2-propenyloxy)benzene, yield 62%; nD23.6 1.5369.

1. customTo a solution prepared
2. additionwas added
3. customa solution prepared
4. additionwas added dropwise under ice cooling
5. stirringAfter stirring at room temperature for 10 hours
6. extractionextracted twice with 50 ml of diethyl ether
7. washwashed with water
8. dry with materialdried over anhydrous magnesium sulfate
9. concentrationconcentrated
10. customto give a crude product