反应详情

Into a mixture of 1.20 g of 2-[2-chloro-4-(3,5difluorophenoxy)phenoxy]ethylamine, 0.81 g of triethylamine and 20 ml of tetrahydrofuran, excesss of carbonyl sulfide gas was introduced with stirring at room temperature for 30 minutes. To the above mixture, there was added dropwise 0.75 g of ethyl iodide, and the resultant mixture was stirred at the same temperature for 24 hours. The reaction mixture was concentrated, and the residue was poured into 100 ml of water and extracted twice with 100 ml of ethyl acetate. The extracts were combined together, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 0.95 g of ethyl 2-[2-chloro-4-(3,5-difluorophenoxy)phenoxy]ethylthiocarbamate. Yield: 61%. nD21 : 1.5707.

1. concentrationThe reaction mixture was concentrated
2. additionthe residue was poured into 100 ml of water
3. extractionextracted twice with 100 ml of ethyl acetate
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure